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

HRID 1973413ノート

反応式

HRID 1973413 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0da4becc20084a17bef8b8cdbb8295e6
出典データセット
uspto-grants-1976_12
特許番号
US03997545

反応ノート

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