Methylamine → 2,6-Difluorophenylacetic acid methylamide

HRID 2372398

反応式

HRID 2372398 の反応式
[CH3:1][NH2:2].[F:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:5]=1[CH2:11][C:12](Cl)=[O:13]>ClCCl>[CH3:1][NH:2][C:12](=[O:13])[CH2:11][C:5]1[C:4]([F:3])=[CH:9][CH:8]=[CH:7][C:6]=1[F:10]

参加物

4

反応物 2

HCID 6329MethylamineHCID 27583212,6-Difluorophenylacetyl chloride

生成物 1

HCID 543845312,6-Difluorophenylacetic acid methylamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

25 ml of methylamine solution (33% in ethanol) are diluted with 90 ml of dichloromethane. While cooling, 9.52 g (50 mmol) of 2,6-difluorophenylacetyl chloride dissolved in 10 ml of dichloromethane are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10°. The reaction mixture is stirred for a further hour at 10° and then extracted three times with water. The organic phase is dried over magnesium sulphate and concentrated. The crude product is recrystallised from dichloromethane/petroleum ether and yields 8.57 g (92.6% of the theoretical yield) of 2,6-difluorophenylacetic acid methylamide of m.p. 163-164°.

後処理

  1. temperatureWhile cooling
  2. additionare added dropwise in such a manner that the temperature of the reaction mixture
  3. customdoes not exceed 10°
  4. extractionextracted three times with water
  5. dry with materialThe organic phase is dried over magnesium sulphate
  6. concentrationconcentrated
  7. customThe crude product is recrystallised from dichloromethane/petroleum ether
  8. customyields 8.57 g (92.6% of the

出典と根拠

ORDレコード
ord-e248cf9073c54ab0922c7b57752b4830
出典データセット
uspto-grants-1992_03
特許番号
US05098922

関連ノート

読み込み中…