IEU CHE ETYL IODUA Phng trnh phan ng:

2P + 3I 2 2PI 3 3CH2CH2OH + PI 3 3CH2CH2 I + H3 PO3

Hoa chat : Etanol khan 15ml (0,246 mol) Iod 15g (0,06 mol) Photpho o 1,5g (0,048 mol) a c lam kho trc trong bnh lam kho tren acid sunfuric Canxi clorua khan ; dung dch NaHSO3, dung dch NaOH Dung cu Bnh cau 100ml ; 1 chiec Bnh cau 50 ml; 2 chiec Bnh tam giac 50 ml (co nut ay); 1 chiec Phieu chiet 125 ml ; 1 chiec Cach tien hanh Cho 1,5 g photpho vao bnh cau 100 ml, them tiep 15ml etanol khan, lac eu. Tiep tuc them tng phan nho cua 15 g iot vao bnh ong thi chuan b 1 chau nc lanh, neu thay bnh phan ng nong len , can nhung bnh phan ng vao nc e lam nguoi bnh. Sau khi cho het iot (khoang 15 phut), them vai vien a bot, un hoi lu hon hp phan ng trong 1,5 gi. Lam nguoi bt hon hp phan ng sau o lap sinh han xuoi e cat chat long ra khoi bnh. Cho chat long vao pheu chiet, ra bang nc e loai ru roi lac vi 1 2 ml natribisunfit ; tiep tuc lac vi dung dch kiem loang cho den khi mat mau iot(1). Chiet lay lp chat long pha di cho vao bnh non, lam kho bang CaCl 2 khan. Chng cat thu c san pham 72 - 730C. (1) Ghi chu : lac hon hp san pham bang dung dich NaHSO3 e loai iot va bang kiem e trung hoa chat long :
I 2 + NaHSO3 + H2O NaHSO4 +2 HI NaHSO4 +2 HI + 3NaOH Na2 SO4 + 2NaI + 3H2 O

Ket qua Lng san pham thu c : ..ml=.mol Lng san pham theo ly thuyet : ..ml =..mol
1

Ghi chu :

Hieu suat san pham so vi ly thuyet: ..% Mau sac san pham Nhiet o soi:

H V TN: L TH THU SANG 2011 LP: HA 3B BI THC HNH S 4

NGY 4 THNG 10 NM

BI 5: IU CH ESTE ISOAMYL AXETAT

1. Phng trnh phn ng (CH3)2CHCH2CH2OH+H2SO4 -> (CH3)2CHCH2CH2OSO3OH +H2O (CH3)2CHCH2CH2OSO3OH + CH3COONa -> (CH3)2CHCH2CH2OCOCH3 + NaHSO4 2. Ha cht:

Alcol isomaylic 1,25g hay 14,8 ml (01,14 mol) Natriacetat khan 12,5g (0,15 mol) Axit sunfuric c(d = 1,84) 12,5g hay 6,75 ml Canxi clorua khan Dung dch natri cacbonat 3. Dng c Bnh cu 100 ml : 1 chic Bnh cu 50 ml : 2 chic Bnh tam gic 50 ml c nt: 1chic B ct thng (sinh hn, nhit k 2000C,ng ni): 1 b Phiu chit 125 ml: 1 chic 4. Tnh cht vt l cc cht
ST T 1 2 3 4 5 TN CHT ts ( 0C) 130 o C 881.4 tnc ( 0C) d (g/ml ) nD20

M m (g/mol (g) ) 88.15 82.03 98,08 130.1 8 105.9 9

n (mol)

V(ml)

Alcol isomaylic Natriacetat

117 0.809 >30 0 1.528 1.464 1,84 78 851 0,871 1,405 9 3 2.54 1.495

Axit sunfuric 290 oC c Este isoamyl 142oC acetat 1600 natri

1,2 5 12, 5 12, 5

01,1 4 0,15

14,8

6,75

cacbonat

5. Cch tin hnh

Cho 12,5 g ancol isoamylic vo bnh cu 100 ml sau sau thm t t 6,75 ml acid sunfuric c vo, va nh va lc sao cho hn hp khng pht nhit qu. Tip tc thm vo hn hp phn ng

12,5 gam natri acetat khan nghin thnh bt, sau lp ng sinh hn ngc v un hi lu hn hp phn ng trn bp cch ct 1500 C trong 1gi.Lm ngui bt hn hp phn ng ri lp ng sinh hn xui , ct cht lng ra . Cho hn hp ct c vo phu chit, chit ly phn trn, ra bng dung dch natri carbonat ri bng nc, lm kh bng canxi clorua. Gn lc ly phn cht lng v chng ct thu ly sn phm 138 140 oC ( khong 12 ml) .Este isoamyl acetat l cht lng khng mu, c mi hoa qu, d420 = 0,8719 ; n20D = 1,4053 ; t0s = 142oC .

6. Kt qu

Lng sn phm thu c:..g= mol Lng sn phm theo l thuyt:g = mol Hiu sut sn phm so vi l thuyt:%

Mu sc ca sn phm: Nhit nng chy:

7. Nhn xt ca gio vin

Khi chng cat giai oan au can phai cat het phan chat long co trong bnh cau do este isoamylic la phan cuoi cung c cat ra ( este iso amylic co nhiet o soi cao hn cac chat long co trong hon hn phan ng) Khi chiet bang ete can phai gi chat pheu chiet Este isoamylic co the ket tinh trong hon hp phan ng mat du ta cha axit hoa no

IEU CHE AIXT XINAMIC Phng trnh phan ng:

C6H5CHO + (CH3CO)2O + K 2 CO3 C6 H5 -CH = CH-COOH + CH3 COOH

Hoa chat. Benzandehit (mi cat lai) 6ml Anhidric acetic(10 ml) Kali cacbonat 5,0g Dung dch NaOH 2 N Than hoat tnh Axit clohidric at Dung cu Bnh cau 250ml ; 1 chiec Coc 400ml ; 2 chiec Bo loc hut chan khong ; 1 bo ua thuy tinh Cach tien hanh Cho vao bnh cau (250,l) 6,0ml benzandehit va cat lai, 10ml anhidric acetic va 5,0 g kali cacbonat khan, nghien mn. Lap sinh han ngc un hoi lu chat long tren bep cach cat 1800C trong 2 gi. Lam nguoi bt roi them vao hon hp phan ng 100ml NaOH 2N (co the un nong tr lai e lam tan het chat ran xuat hien trong bnh). Lam nguoi hon hp phan ng en nhiet o phong roi chuyen vao pheu chiet, chiet bang 20ml ete. Them vao phan dung dch thu c 1g than hoat tnh, un soi 10 15 phut roi loc. Co phan nc loc en khoang 130ml, e nguoi va acid hoa bang HCl ac en moi trng acid. Loc acid xinamic tach ra tren pheu Bucne, ra san pham bang nc va say 105 1100C thu c khoang 4,0 g san pham. San pham tho co nhiet o nong chay khoang 1280C. Axit xinamic la chat ket tinh mau trang, nhiet o nong chay t0nc = 1330C KET QUA Lng san pham thu c ..g =mol Lng san pham theo ly thuyet :..g = .mol Hieu suat pham so vi ly thuyet: ..% Mau sac cua san pham: Nhiet o nong chay: NHAN XET CUA GIAO VIEN :

IEU CHE AXETANILIT Phng trnh phan ng:

C6H5NH2 + (CH3CO)2O C6 H5 NHCOCH3 + CH3 COOH

Hoa chat : Anilin mi cat ; 2,3 g (0,025 mol) Anhirit acetic 3 ml(0,03 mol) Axit clohidric ac(d = 1,19): 2 ml Natri acetat tinh the : 3,8g Dung cu Coc 250 ml:2 chiec Bo loc hut chan khong ua thuy tinh Cach tien hanh Cho 2 ml axit clohidric vao coc 250 ml co cha san 60 ml nc, khuay roi them 2,3 g anilin. Neu dung dch co mau th them 0,5 g than hoat tnh, khuay trong 5 phut va loc. un nong dung dch khong mau cho en 50 0C, cho them 3 ml anhidric acetic va khuay cho en khi tan hoan toan. o nhanh hon hp phan ng vao dung dch natri acetat cha 3,8g natri acetat trong 12ml nc ; khuay manh roi ngam trong nc lanh cho ti khi acetanilit tach ra hoan toan. Loc tren pheu Bucne, ra bang nc va ket tinh lai trong nc ru thu c khoang 2,7 g san pham. Axetanlit la chat ket tinh mau trang, tan tot trong ru clorofom, t tan trong nc nong chay 1140C. Ket qua Lng san pham thu c:g =.mol Lng san pham theo ly huyet:..g = .mol Hieu suat san pham so vi ly thuyet: ..% Mau sac cua san pham: Nhiet o nong chay;

NHAN XET CUA GIAO VIEN

IEU CHE AXIT BENZOIC Phng trnh phan ng:

C6H5CH3 + KMnO4 C6 H5COOK + MnO2 + KOH + H2 O C6H5COOK + HCl C6 H5COOH + KCl

Hoa chat : Toluen 2ghay 2,5 ml (0,02 mol) Kali pemanganat 6,8g (0,04 mol) Acid clohidric 1:1 Axit oxalic (tinh the) Dung cu Bnh cau 100ml: 1 chiec: Coc 250 ml; 2 chiec Bo loc hut chan khong ua thuy tinh Cach tien hanh Hoa tan 6,8 g KMnO4 trong 75 ml nc roi chuyen vao bnh cau 100ml ; them tiap61 vao bnh 2,5 ml toluen va vai vien a bot roi lap sinh han ngc, un hoi lu hon hp trong 2 gi. Trong qua tnh un can lac bnh. Neu sau phan ng dung dch con mau hong th them vai hat tinh the axit oxalic e oxi hoa not kali pemanganat con d ( lu y ch them tinh the axit oxalic khi ket thuc phan ng). Loc bo dioxit mangan tren pheu Bucne, rua lai bang 1 t nc nong. Co nc loc cho an khi the tch con lai khoang 20 25 ml. e nguoi, roi acid hoa bang axit clohidric (1:1), acid benzoic tacg1 ra di dang chat ran mau trang hnh vay; loc; ra bang nc lanh, lam kho trong khong kh thu c 2 g san pham. Axit benzoic la chat ket tinh khong mau, kho tan trong nc lanh, tan tot trong ancol, clorofo nong chay 122,30C Ket qua Lng san pham thu c:g =.mol Lng san pham theo ly huyet:..g = .mol Hieu suat san pham so vi ly thuyet: ..% Mau sac cua san pham: Nhiet o nong chay;

NHAN XET CUA GIAO VIEN

Hoa chat : Dung cu Ket qua Cach tien hanh Ff ghh