Pyridine → methyl 2-(acetylamino)-5-chloro-3-thiophenecarboxylate

HRID 1973413노트

반응식

HRID 1973413 반응식
[C:1]([NH:4][C:5]1[S:6][CH:7]=[CH:8][C:9]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:3])[CH3:2].C(Cl)(Cl)[Cl:15].N1C=CC=CC=1.ClCl>C(Cl)(Cl)(Cl)Cl>[C:1]([NH:4][C:5]1[S:6][C:7]([Cl:15])=[CH:8][C:9]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 6212ChloroformHCID 24526ChlorineHCID 2808565Methyl 2-acetamidothiophene-3-carboxylate

생성물 1

HCID 818981methyl 2-(acetylamino)-5-chloro-3-thiophenecarboxylate

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To a stirred solution of 4 parts of methyl 2-acetamidothiophene-3-carboxylate in a mixture of 80 parts by volume of chloroform and 12 parts by volume of pyridine, 20 parts by volume of a 10% (W/V) solution of chlorine in carbon tetrachloride is added dropwise. After stirring for further 30 minutes, the mixture is washed with an aqueous sodium bicarbonate solution and, then, with water. Evaporation of the solvent, and recrystallization of the residue from methanol gives methyl 2-acetamido-5-chlorothiophene-3-carboxylate as crystals. Colorless needles, melting point: 110°-110.5° C.

후처리

  1. additionis added dropwise
  2. washthe mixture is washed with an aqueous sodium bicarbonate solution
  3. customEvaporation of the solvent, and recrystallization of the residue from methanol

출처 및 근거

ORD 기록
ord-0da4becc20084a17bef8b8cdbb8295e6
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03997545

반응 노트

불러오는 중…