bao cao huu co 1

GVHD: Mai Th Thy Lam

SVTH: Nhm 8 DA09HH

Nhn xt ca gio vin

Bo co thc hnh hu c I

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SVTH: Nhm 8 DA09HH

PHN TCH NH TNH CC NHM CHC HU CI. C s l thuyt

nh tnh cc nhm chc hu c.II.

Dng c v ha cht Dng c: ng nghim Pipet nha Gi ng ng nghim Ha cht: Dung dch K2Cr2O7 10% Dung dch NaOH 10% Dung dch NaOH 2N Ethanol Acetone Tin trnh th nghim - Dung dch H2SO4 10% - Dung dch KMnO4 1% - Dung dch I2 trong KI - Isoamylic - Thuc th Lucas - Beaker - n cn - Kp ng nghim

1.-

2.-

III.

1. Alcol Phn ng oxi ha Ly 4 ng nghim, cho vo mi ng 1ml ethanol ri ln lt thm vo: ng 1: 1ml dung dch K2Cr2O7 10% v 3 git H2SO4 10%, lc mnh, ta thy kt ta trng: K2Cr2O7 + H2SO4 + C2H5OH K2SO4 + Cr2(SO4)3 + 7H2O + 3CH3CHO ng 2: 1 git dung dch KMnO4 1% v mt git H2SO4 10%, lc u, th ta li thy dung dch chuyn sang mu vng nu cam. 2 KMnO4 + H2SO4 Mn2O7 + H2O + K2SO4 Mn2O7 2MnO2 + O3 C2H5OH CH3CHO (tc dng vi O3) Hay 2KMnO4 + 2H2SO4 + 3C2H5OH 3CH3COOH + K2SO4 + MnSO4 +5H2OBo co thc hnh hu c I Trang 2


SVTH: Nhm 8 DA09HH

ng 3: 1 git dung dch KMnO4 1% v 1 git NaOH 10%, lc u s thy kt ta vng mu nu nht. 2KMnO4 + 2NaOH + C2H5OH CH3COOH + K2MnO4 + Na2MnO4 + 2H2O ng 4: 5 git dung dch KMnO4 1% un nng mt lc c hin tng kt ta nu. 3 C2H5OH + 4 KMnO4 3 CH3COOH + 4 MnO2 + 4 KOH 2. iu ch Iodoform t etylic v aceton A. iodoform - thuc vng, CHI3. Tinh th mu vng, mi kh chu; d b thng hoa; tan trong clorofom. iu ch bng cch cho dung dch hipoio (dung dch iot trong xt (NaOH) hoc natri cacbonat (Na2CO3) tc dng vi etanol hoc axeton. Phn ng to thnh I dng nh lng etanol, axeton, cc metylxeton, axetanehit, vv. I c dng lm cht st trng. a) iu ch t alcol ng nghim 0.5ml etanol; 1,5ml dung dch I2 trong KI v 1,5ml NaOH 2N. Lc v un nh cho n khi dung dch xut hin kt ta vn c (khng si); lm lnh vi vi nc, quan st kt ta. C ch phn ng

b) iu ch Iodoform Cho 2ml dung dch I2 trong KI v 2ml NaOH 2N vi 0.5ml axeton v lc nh ta thy xut hin kt ta trng c nu thm d th kt ta tan to thnh dung dch trong.


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SVTH: Nhm 8 DA09HH

3. Nhn bit bc ru bng thuc th Lucas ng 1: 1ml etanol v 1ml thuc th Lucas thy hin tng si bt kh v ta nhit. ng 2: 1ml iso anylic v 1ml thuc th Lucas thy hin tng si bt, dung dch c hin tng tch lp nh do Isoamylic tc dng vi thuc th Lucas bng cch chuyn v to C+ bn, to dn xut Clo tng ng nhng tc phn ng xy ra chm ng 3 :1ml cyclohexanol v 1ml thuc th Lucas, lc u s xut hin s tch lp sau tan. * Thuc th Lucas (dung dch HCl + ZnCl2) c dng phn bit cc ru bc mt, bc hai, bc ba. Cc ru t hn 6 nguyn t C trong phn t tan trong thuc th. -

Ru no m tc dng vi thuc th Lucas thy dung dch c ngay (do to dn xut Clo t tan) th l ru bc 3. Ru no m tc dng vi thuc th Lucas vi pht sau (khong 5 pht) mi thy dung dch c (do to dn xut Clo t tan nhng chm hn) th l ru bc 2.

-

Ru no m tc dng vi thuc th Lucas m khng ty dung dch c th l ru bc mt (do tc to RCH2Cl chm hn, cn un nng phn ng mi xy ra).


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SVTH: Nhm 8 DA09HH

Bi 1: PHN NG OXI HA KHI.

C s l thuyt

iu ch acid Benzoic da trn phn ng oxi ha-kh ca KMnO4 vi Toluene. II. 1. -

Dng c v ha cht Dng c: Bnh cu 250ml Beaker 500ml a thy tinh bt Pipet nha Ha cht: KMnO4 rn Dung dch H2SO4 20% Dung dch H2O2 Tin trnh th nghim - Toluen - Na2CO3 tinh th - H thng un hon lu - Beaker 100ml - H thng lc p sut thp - Bp in

2.-

III.

- Cho vo bnh cu 250ml 12g KMnO4 v 80ml nc, vi vin bt. em un nh v khuy u cho tan ht KMnO4 cho tan ht trong 10 pht. - ngui v thm vo bnh cu 5ml toluene, 2g Na2CO3, gn bnh cu vo h thng un hon lu, un nh hn hp cho n khi dung dch chuyn mu sm (khong 60 pht) phi thng xuyn lc nh bnh cu. Lc ny trong bnh cu s xy ra phn ng: 6C6H5CH3 + 2KMnO4 C6H5COOK + 2MnO2 + KOH + H2O - ngui sao cho hn hp vo mt becher 500ml. - Thm vo becher 100ml H2SO4 20%, khuy tht u bng a thy tinh, C6H5COOK tc dng vi H2SO4 to thnh acid benzoic. C6H5COOK + H2SO4 2C6H5COOH + K2SO4Bo co thc hnh hu c I Trang 5


SVTH: Nhm 8 DA09HH

- loi KMnO4 v H2SO4 d ta cho tng lng nh H2O2 va thm va khuy cho n khi dung dch mt mu (chuyn sang mu trng c) th ngng. H2O2 + KMnO4 + H2SO4 O2 + K2SO4 + MnSO4 + H2O - ngui becher v lm lnh dung dch trong chu nc , acid benzoic s kt tinh, lc kh sn phm di p sut km. - Cho axit benzoic va lc kh vo becher 100ml cha mt t nc, un si. Nu axit benzoic cha tan ht, thm nc cho n khi tinh th ny tan hon ton. - ngui t t, acid benzoic s kt tinh thnh tinh th hnh kim. Lc kh sn phm di p sut km.IV.

Kt qu th nghim

Thu c Acid Benzoic kt tinh c khi lng l 0.783g Theo phng trnh phn ng th: Khi lng toluen tham gia phn ng l = V*D = 5* 0.8669 = 4.3345g S mol ca toluen = m/M = 4.3345/92.14 =0.047mol Da vo phng trnh phn ng S mol ca Acid Benzoic l 0.0157mol Khi lng Acid Benzoic thu c l 1.9gam. Vy hiu sut ca th nghim l 41% * Acid benzoic l tinh th hnh kim khng mu, dng bo qun thc phm, keo dnh, sn xut phm nhum, dc phm v cht thm. Trong y hc lm thuc st trng, dit nm.


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SVTH: Nhm 8 DA09HH

BI 2 : NG PHN CIS TRANSI.

C s l thuyt

Thy c s chuyn i qua li gia hai ng phn ca nhau l axit Maleic v axit Fumaric v s khc bit v tnh cht vt l ca chng.II.

Dng c v ha cht Dng c: - H thng lc p sut thp - Bp in

1.

- Erlen 250ml - H thng un hon lu

2. -

Pipet nha Ha cht: Anhydric Maleic Acid HCl m

III.

Tin trnh th nghim iu ch acid Maleic Cho 10g Anhydric Maleic vo Erlen 250ml vi 10ml nc v em un si. Khi em lc di p sut km ly ring tinh th axit Maleic Ch : khng ra tinh th axit Maleic trn phu v axit Maleic tan nhiu trong Phng trnh:O O O O OH O OH

1.-

Anhydric Maleic tan ht, em lm lnh di vi nc, axit Maleic s kt tinh. nc. -


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SVTH: Nhm 8 DA09HH

2. -

iu ch acid Fumaric phn dung dch qua lc vo Erlen 250ml, thm vo 10ml HCl m c.

Gn ng hon lu v un nh hn hp trong 10 pht. Nhng tinh th axit Fumaric s hin ra trong dung dch nng. ngui hn hp ri em lc di p sut km, sau kt tinh li axit Fumaric Phng trnh:O OH O O

trong dung dch HCl 1M.

HClOH HO O

OH

Phng trnh tng qut chuyn ha qua li gia acid Maleic v FumaricO O O O O OH O

HClOH HO O

OH

IV.-

Kt qu th nghim Tinh th acid Maleic c mu trng, khi lng l 4,761g, t s=135oC, d=1.59g/cm3, Tinh th acid Fumaric c khi lng l 1,972g, tan km hn nhiu so vi acid

tan: 78g/100ml nc 25OC.-

Maleic: 0.63g/100ml nc 25oC, c tnc = 278oC.


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SVTH: Nhm 8 DA09HH

BI 3: PHN NG ALKYL HA IU CH ETER NAPTHYL METHYL (NEROLIN)I. Mc chOH O

iu ch eter Naphthyl methyl (Nerolin) t Naphtol v ru Methylic.H2SO4, t0C

+

CH3OH

II.

Dng c v ha cht - a thy tinh - Bp gia nhit - My ht chn khng

1. Dng c - Erlen 250ml - Beaker 50ml - Beaker 500ml 2. Ha cht - Naphtol - H2SO4 c III. Tin trnh thc hnh - Ru metylic - NaOH 5%

Cho vo erlen 250ml 15gam Naphtol v 20ml ru etylic, lc k bnh cho ha tan Naphtol. Sau thm 3ml H2SO4 c vo (hn hp pht nhit mnh). un cch thy trong 2 gi. Sau khi un rt dung dch m vo beaker 500ml cha 45ml dung dch NaOH 5% un nng ln 500C. Trong trng hp ny Nerolin lng xung di dng du en v c khuy mnh trn ln vi dung dch kim cho n khi ha rn hon ton ( ngn Nenrolin ha rn ngay lp tc cn phi un nng dung dch kim trong khi rt hn hp phn ng vo v phi un cch thy bnh tam gic).


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SVTH: Nhm 8 DA09HH

Cht kt ta c mu vng nu, c lc v x l ln na vi NaOH ging lng ban u. Ra Nerolin vi nc cho n khi th giy qu khng cn phn ng kim. Sy nhit khng qu 500C. C ch phn ng phn t 2- Naphthol hiu ng ht electron 2 nhn thm i vi phn t Oxi v s ht electron oxi lm cho nguyn t hir rt linh ng.O H

Phn t methanol, mt phn do hiu ng y electron ca nhm CH3 mt phn do Oxi ht electron ca hiro cng lm cho hir linh ng.H3CO H

C ch phn ng nh sau:O HH O C H2 O H

H2C

O

H

O CH3

H O

+ Ngoi ra cn c nhng sn phm ph nh:O

H

O

Di naphthyl eter

Dimethyl eter

Cc sn phm ny s c tinh ch bng NaOH v ra li bng nc. IV. Kt qu th nghim

Kt thc phn ng ta thu c Naphthyl methyl vi khi lng l 9.9738gBo co thc hnh hu c I Trang 10

GVHD: Mai Th Thy Lam Theo l thuyt ta c: S mol ca Naphtol tham gia phn ng l m/M = 15/144.17 = 0.104 mol S mol ca Naphthyl methyl l 0.104mol

SVTH: Nhm 8 DA09HH

Khi lng ca Naphthyl methyl thu c l 16.45g Vy hiu sut ca phn ng l 60%

BI 4: IU CH ESTER ACETAT ISOAMYLI. Mc ch iu ch ester acetate isoamyl (c mi du chui) bng phng php un hon lu alcol isoamylic vi acid acetic, c H2SO4 c lm cht xc tc:CH3COOH + (CH3)2CHCH2CH2OH alcol isoamylicH2SO4, to

CH3COOCH2CH2CH(CH3)2 + H2O ester acetate isoamyl

II.

C s l thuyt Este, mt cht c nhm chc -COO- , a s l hp phn chnh ca hng liu hoa

qu nh este focmiate etyl c mi ru rum, este acetate isoamil c mi chui chn, este butyrate c mi nho Este c th c tng hp bng cc phn ng ca acid cacboxylic v ru vi s hin din ca acid sulfuric m c, hidro Clorua, acid p- toluen sulfomic hoc nha trao i ion. Trong iu kin hin ti ca phng th nghim, ta thc hin phn ng ester ha vi acid sulfuric m c. III. 1. Dng c v ha cht Dng c - Phu chitTrang 11

- Bnh cu dung tch 100mlBo co thc hnh hu c I

GVHD: Mai Th Thy Lam - Pipet 10ml - bt 2. Ha cht

SVTH: Nhm 8 DA09HH - ng nghim

- Ru isoamylic - Axit sunfuric - NaHCO3 IV. 1. Tin hnh th nghim iu ch ester acetat isoamyl

- Na2SO4 khan - Axit axetic

Cho hn hp gm 15ml ru isoamylic vo 10ml acid acetic vo bnh cu dung tch 100ml. Sau thm t t tng git n ht 1ml Axit sunfuric m c, thm vo mt t bt. Gn bnh cu vo h thng hon lu v un cch thy trong 45 pht. ngui, sn phm thu c gm acetat ethyl th ln axit, ru v nc. C ch phn ng: Xy ra theo c ch phn ng th i nhn, cc bc phn ng xy ra theo trnh t s sau:H O H OH OO H H O O H

H O OH O

O HO O H H

H O H

O


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SVTH: Nhm 8 DA09HH

O H O O O H H

O

O

+H

OH

+

H O H

2.

Tinh ch sn phm Cho hn hp vo bnh chit, thm t t dung dch NaHCO 3 bo ha n ht bt

kh, va cho va lc, n khi dung dch tch thnh 2 lp r rt. NaHCO 3 bo ha dng trong th nghim trung ha lng acid d, to mi trng trung tnh. C th dng H2O thay NaHCO3. CH3COOH + NaHCO3 CH3COONa + CO2 + H2O Ly ester trn vo bnh tam gic, thm vo 1g Na 2SO4 khan, lc nh yn, thu c sn phm l cht lng khng mu, c mi thm ca du chui. Na2SO4 khan c tc dng ht nc cn ln trong ester. 3. Kim nghim sn phm Cho vo ng nghim: vi git ester + vi ht tinh th NH2OH.HCl + trung ha bng 1ml NaOH 10%. un si lm lnh + thm t t dung dch HCl long + thm vi git FeCl3. * Hin tng: Dung dch c mu . * Gii thch: Ester acetate isoamyl tc dng vi hidroxylamin to thnh acid hidroxamic:


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GVHD: Mai Th Thy LamO

SVTH: Nhm 8 DA09HHO

R

OR'

+ H2N-OH

R

NHOH

+ R'-OH

Sau , FeCl3 c cho vo acid hidroxamic, chng tc dng vi nhau to ra hp cht [R-OONH]3 Fe c mu.O O NHOH

R

+ FeCl3

R

NHO-

3

Fe

+ 3 HCl

Nu cht kho st l ester ca acid cacboxylic th mu ca dung dch s chuyn thnh mu hoc tm. Hin tng quan st c l mu hng chng t sn phm thu c l ester acetat isoamyl. V. Kt qu th nghim

S mol ca ru isoamylic l: 0,1705mol S mol ca acetic acid l: 0,1667mol S mol ca ester acetate isomyl : 0,1667mol Khi lng ester theo l thuyt : 21,671g.

BI 5: IU CH NAPHTHYL ACETATEI. C s l thuyt

Phn ng ester ha l phn ng gia acid hu c v ancol c mt xc tc l acid mnh nh H2SO4 hoc HCl y l phn ng thun nghch, xy ra theo hai chiu. C th s dng anhydride thay axit iu ch este, phn ng xy ra theo mt chiu v khng cn phi s dng xc tc. i vi cc phn t c vng thm nh naphthol tn ti hiu ng ht in t rt mnh ca nhn thm chnh v vy khng th tham gia trc tip phn ng este ha nh


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SVTH: Nhm 8 DA09HH

ancol vi acid carboxylic. M phi to thnh mui vi mt kim trc khi tham gia phn ng este ha. Ar OH + NaOH ArONa + H2O C ch ca phn ng ester ha s dng xc tc:

II. 1.- Cn

Dng c v ha cht Dng c - ng sinh hn - Bp in - T sy

- Bnh cu y trn 500 ml

- Lc ht chn khng

2.

Ha cht - Anhidric Acetic - Dung dch NaOH 10%

- -Naphtol - Ethanol

-

Nc


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GVHD: Mai Th Thy Lam III. Tin hnh th nghim

SVTH: Nhm 8 DA09HH

Ha tan 5g -naphtol vo 25ml dung dch NaOH 10% vo bnh cu y trn dung tch 500ml. Thm 20g nc vn v 6g anhydric acetic vo dung dch, lp ng sinh hn, un nh trong 30 pht. ngui, lc, ra bng nc v sy kh. Kt tinh li trong ethanol. em sy sn phm trong t sy khong 20 pht 40-50 oC . Cn tnh hiu sut. C th chia qu trnh iu ch lm 3 giai on: Giai on 1: chuyn naphtol sang dng naphtolat. Giai on 2: este ha bng anhydrit axetic. Giai on 3: kt tinh li trong ethanol. Giai on 1: chuyn naphtol sang dng naphtolat Ha tan 5g -naphtol vo 25ml dung dch NaOH 10% vo bnh cu y trn dung tch 500ml. Ti y xy ra phn ng to thnh naphtolat sau y: -

+HO

NaOHNa+ O

+

H2O

beta-naphthol

sodium beta-naphtholate

Trong phn t do c cha 2 nhn thm, nn hiu ng ht in t v pha nhn l rt mnh nn tnh acid ca - naphtol mnh hn ancol v nc chnh v vy - naphtol khng th tham gia phn ng este ha trc tip vi acid cacboxylic m phi to thnh mui - naphtolat trc. y l phn ng c bn cht l phn ng trung ha gia axit v baz trong - naphtol th hin tnh axit. Qu trnh ny nhm lm tng mt in tch gip to iu kin cho phn ng este din ra. Giai on 2: ester ha bng anhydric acetic Sau khi - naphtol ha tan ht vo trong NaOH, tip tc cho lnh (200g) vo bnh cu v cho vo 6g anhydric axetic vo, lc bnh cu lin tc trong 30. Sau lp ng sinh hn un trong 30 pht.Bo co thc hnh hu c I Trang 16

GVHD: Mai Th Thy Lam Lc ly ta, ra kt ta bng nc. Phn ng xy ra trong giai on ny l:

SVTH: Nhm 8 DA09HH

O

O

O

+ CH3COONaO

+Na+O O

sodium beta-naphtholate

acetic anhydride

beta-naphthyl acetate

C ch phn ng este ha gia Anhydrit axetic v - naphtolat : gian.

Trc ht nhm carbonyl ca anhydrit c proton ha, hnh thnh cation trung

Tip theo l giai on tn cng ca nguyn t oxygen trn phn t - naphtolat

vo cation ny, km theo giai on proton ha v to thnh CH3COONa. Cui cng l giai on tch proton ti sinh xc tc, hnh thnh sn phm este.

Ngi ta s dng anhydric axetic nhm phn ng din ra mt chiu v khng cn xc tc v c tnh axit mnh hn axit cacboxylic. Trn thc t, vic dng anhydric axetic l d so vi lng va vi l thuyt dng trong phn ng trn, nguyn nhn l trung ha NaOH cn d. Do , khi kt ta va to ra c mu trng l do c ln tp cht CH3COONa theo phn ng: (CH3CO)2O + 2NaOH 2CH3COONa + H2O cho vo dng lm lnh dung dch, to iu kin cho tinh th tch ra nhanh hn. Lc tch kt ta ra khi dung dch, v ra bng nc ct loi bt dung dch cn bm trong ta. Giai on 3: kt tinh trong ethanol Do trong kt ta va lc vn cn tp cht nn phi kt tinh li nhm tinh ch sn phm. Cho kt ta va lc vo dung dch ethanol, sau un nh trn bp in.


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SVTH: Nhm 8 DA09HH

Sau lm lnh trong 30 pht, em lc di p sut thp v sy nhit khng vt qu 50oC nu khng kt ta s b nng chy.

IV.

Kt qu th nghim -

S mol anhydric acetic : 0,0588mol S mol naphthol : 0,0347mol S mol naphthyl acetate theo l thuyt l : 0,0347mol. Khi lng naphthyl acetate theo l thuyt l : 6,4542g Khi lng naphthyl acetate thc t thu c l: 5,15g Hiu sut ca qu trnh iu ch naphthyl acetate l : 79,79%.

-

BI 6: IU CH ASPIRINI. Mc ch

Aspirin l mt trong ba loi thuc gim au c s dng rng ri nht nn vic iu ch aspirin l mt ng dng quan trng trong y hc v cuc sng. Nn vic iu ch aspirin l mt vic quan trng trong cuc sng ca con ngi.

II.

C S L Thuyt

Aspirin hay cn gi l acid acetyl salisylic l mt loi ester. L cht kt tinh khng mu, tan t trong nc nhng tan nhiu trong ru. V th m ru c dng kt tinh li aspirin. Phn ng iu ch aspirin chnh l phn ng este ha gia acid salicylic v anhydric acetic trong mi trng acid. Phn t ca acid salicylic cha hai nhm chc trong c mt nhm chc l phenol v mt nhm chc l acid cacboxylic. V vy n c th toBo co thc hnh hu c I Trang 18


SVTH: Nhm 8 DA09HH

thnh mt este vi vai tr ca mt acol phn ng acid acetic to thnh acetyl salisylic. Tuy nhin, aspirin thng c u ch bng cch dng anhyric acetic hot ng hn thay v acid acetic. Phng trnh phn ng:COOH OH + CH3 C O Acid salysilic O C O Acid acetyl salisilic (Aspirin) acid acetic CH3 COOH OCOCH3 + CH3COOH

Anhydric acetic

Phn ng este ha l phn ng thun nghch. V vy, bnh thng khi t trng thi cn bng th hiu sut khng vt qu 66,7%. Tuy nhin c th chuyn dch cn bng theo chiu thun bng cch : Dng d mt trong cc cht tham gia phn ng, thng dng d ancol. Gim nng cht to thnh trong phn ng. Dng xc tc thc y phn ng nh axit sunfuric, nha trao i ion, cc

mui axit kim loi C ch phn ng:

H+

CH3 C O

.. O

C O

CH3

CH3 C O

+ O H

C O

CH3

-OH

CH3 C O COOH O

OH

+C O

CH3

+

CH3 C O

OH

H + CH3 C O .. OH

COOH O+ CH3 C O + OH2

COOH O C O CH3

III.

Dng c v ha chtTrang 19


GVHD: Mai Th Thy Lam 1. Dng c

SVTH: Nhm 8 DA09HH

- Erlen 100ml - ng nghim - Bp in 2. Ha cht

- Beaker 250 ml - ng nh git - Lc ht chn khng

- Acid Salicylic - Acid H2SO4 m c - Dung dch FeCl3 10%

- Anhidric Acetic - Ethanol - Nc ct

IV.

Tin trnh thc hnh

Cho vo erlen 100ml 5g acid salicylic, 7,5g anhydric acetic v 3 git H2SO4 m c. em erlen un cch thy nh trong 30 pht, ngui v thm vo 100ml nc, khuy k xong em lc di p sut km thu c aspirin th. Ha tan aspirin th trong mt lng ti thiu etanol nng (dung dch trong sut, nu cha tan dng ng nh git thm t t cho n khi tan hon ton), sau thm nc t t n khi xut hin kt ta bn, li thm vi git etanol n khi kt ta tan ht. ngui dung dch t t, aspirin s kt tinh thnh tinh th hnh kim. Lc kh sn phm di p sut km. Cn v tnh hiu sut. Di y l s tm tt qu trnh iu ch aspirin:

5g acid salicylic H2SO4

7,5g anhydric acetic

Tinh th aspirin Sy Lc p sut thp Tinh th Lm ngui Dung dch Tinh th

un khuy u (50oC 60oC) Lm ngui Ester + tp cht Thm nc Dung dch hu th Bo co thc hnh + tinh c I

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SVTH: Nhm 8 DA09HH

Lc p sut thp

Ethanol nng

Kim nghim sn phm: Ly 2 ng nghim: ng 1: cho vo vi tinh th acid salicylic. ng 2: cho vo vi tinh th aspirin va iu ch. Ln lt cho 1ml ru etylic v vi git FeCl3 10% vo tng ng lc k. Hin tng: ng 1: dung dch mu tm. ng 2: dung dch mu nu en. V. Kt qu

S mol ca acid salicylic : 0,0362mol. S mol ca anhidric acetic : 0,0735mol. S mol ca aspirin theo l thuyt l 0,0362mol. Khi lng aspirin theo l thuyt l : 6,516g. Khi lng aspirin iu ch thc t l 4,64g. Hiu sut ca qu trnh iu ch aspirin l: (4,94/6,516) * 100 = 71,21%

BI 7: IU CH ACETANILIDEI. C s l thuyt


Trang 21


SVTH: Nhm 8 DA09HH

Phn ng axyl ha l qu trnh gn nhm axyl vo phn t hp cht hu c, thng bng phn ng th hidro ca hidrocacbon thm v hidro ca mt vi nhm chc (-OH, -NH2,..). Phn ng acyl ha l phn ng c trng ca amin thm. Phn ng trong khng nhng cn amine c tnh base mnh m cn i hi trn nguyn t nitrogen phi c proton. Tc nhn acyl ha thng dng: CH3COCl, (CH3CO)2O, hay CH3COOH. mnh yu ca tc nhn acetyl nh hng ln n kh nng v tc phn ng V d: mun iu ch acetanilide t aniline. Trong trng hp ny c th s dng tc nhn acyl ha l acetic acid, tuy nhin phn ng s thun nghch v tc phn ng chm hn nhiu so vi trng hp acetyl chloride hoc acetic anhydrire. II. 1. Ha cht v dng c Dng c - Beaker 250ml - ng ong 20ml - Bp in

- Beaker 500ml - Lc ht chn khng - Cn - a thy tinh, pipet nha 2. Ha cht

- Anilin - Anhidric Acetic - Than hot tnh III.Tin hnh th nghim

- Axit HCl c - Natri Acetat - Nc ct

Cho 250ml nc vo cc 500ml, thm vo 8.5 ml acid HCl c v va khuy va thm tip vo 9ml Anilin. Khi Anilin tan ht, em dung dch un nng n 500C ri thm vo 12.5 ml Anhidric Acetic v khuy u cho tan ht. Ha tan sn 15g Natri Acetat trong trong 50ml nc, 2 dung dch vo nhau, khuy mnh ri ngm dung dch trong nc lnh cho n khi Acetanilit tch ra hon ton.Bo co thc hnh hu c I Trang 22


SVTH: Nhm 8 DA09HH

Ch : vic cho HCl c vo dung dch c tc dng to mi trng cho sn phm khng b thy phn trong nc, ng thi khng cht bn i vo sn phm. Phn ng iu ch Acetanilit thuc phn ng axyl ha, c th phn ra cc giai on sau: Giai on 1: acyl ha aniline bng anhydrit axetic Giai on 2: acyl ha aniline bng acid axetic. Phng trnh phn ng:

III.

Kt qu th nghim

S mol ca aniline l : 0,0989mol S mol ca anhydric acetic l : 0,123mol S mol ca acetanilide : 0,0989mol Khi lng ca acetanilide theo l thuyt: 13,3515g Khi lng acetanilide thc t thu c l: 8,763g Hiu sut ca qu trnh: 65,63%


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bao cao huu co 1

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