Water → N-[2-(3-methyl-4-methoxyphenyl)ethyl]-3-(4-chlorophenyl)propionamide

HRID 893320

反応式

HRID 893320 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH2:10][CH2:11][NH2:12])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][C:22](O)=[O:23])=[CH:16][CH:15]=1.O>C1(C)C(C)=CC=CC=1>[CH3:1][C:2]1[CH:3]=[C:4]([CH2:10][CH2:11][NH:12][C:22](=[O:23])[CH2:21][CH2:20][C:17]2[CH:18]=[CH:19][C:14]([Cl:13])=[CH:15][CH:16]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]

参加物

5

反応物 3

HCID 962WaterHCID 123137beta-(p-Chlorophenyl)propionic acidHCID 64846602-(4-Methoxy-3-methylphenyl)ethan-1-amine

生成物 1

HCID 19892235N-[2-(3-methyl-4-methoxyphenyl)ethyl]-3-(4-chlorophenyl)propionamide収率 80.1%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

Heat a solution of 2-(3-methyl-4-methoxyphenyl)ethylamine (64.4 g) and 3-(4-chlorophenyl)-propionic acid (70.2 g) in xylene (600 mL) at reflux over a Dean-Stark trap for 5.5 h. Pour the hot reaction mixture into water an allow to stand overnight. Filter to collect the solid and recrystallize from ethanol to give N-[2-(3-methyl-4-methoxyphenyl)ethyl]-3-(4-chlorophenyl)propionamide (101.1 g), mp=142°-144° C.

後処理

  1. temperatureat reflux over a Dean-Stark trap for 5.5 h
  2. filtrationFilter
  3. customto collect the solid
  4. customrecrystallize from ethanol

出典と根拠

ORDレコード
ord-d59382d05ed643019d118244af46137a
出典データセット
uspto-grants-1992_06
特許番号
US05124337

関連ノート

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