2-Thiopheneacetyl chloride → Methyl 4-chloro-5-nitro-2-(2-(thiophen-2-yl)acetamido)benzoate

HRID 1275589ノート

反応式

HRID 1275589 の反応式
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]([Cl:13])=[CH:6][C:5]=1[NH2:14].[S:16]1[CH:20]=[CH:19][CH:18]=[C:17]1[CH2:21][C:22](Cl)=[O:23]>>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]([Cl:13])=[CH:6][C:5]=1[NH:14][C:22](=[O:23])[CH2:21][C:17]1[S:16][CH:20]=[CH:19][CH:18]=1

参加物

3

反応物 2

HCID 1623622-Thiopheneacetyl chlorideHCID 15895692Methyl 2-amino-4-chloro-5-nitrobenzoate

生成物 1

HCID 54055967Methyl 4-chloro-5-nitro-2-(2-(thiophen-2-yl)acetamido)benzoate収率 67.6%

実験手順

To a suspension of 2-amino-4-chloro-5-nitrobenzoic acid methyl ester (221 mg in 2.5 mL of dry 1,2-dichloroethane) was added a solution of thiophen-2-yl-acetyl chloride (169 mg in 3.0 mL dry 1,2-dichloroethane) and the mixture heated at reflux on an oil bath. After 18 hours, the reaction was cooled and the solvent removed in vacuo. Recrystallization of the crude product from methanol gave the title compound (230 mg).

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux on an oil bath
  3. temperaturethe reaction was cooled
  4. customthe solvent removed in vacuo
  5. customRecrystallization of the crude product from methanol

出典と根拠

ORDレコード
ord-9703dbf67a7b47bb91410fcd9fcf56fd
出典データセット
uspto-grants-2000_12
特許番号
US06162813

反応ノート

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