4-Chlorobenzylamine hydrochloride → HCID 178512103、化合物

HRID 413748

反応式

HRID 413748 の反応式
[NH:1]([C:4]1[CH:5]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:8][CH:9]=1)[C:2]#[N:3].Cl.[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][NH2:21])=[CH:18][CH:17]=1>ClCCl>[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][NH:21][C:2]([NH:1][C:4]2[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:11])([F:12])[F:13])[CH:5]=2)=[NH:3])=[CH:18][CH:17]=1

参加物

4

反応物 2

HCID 4584434-Chlorobenzylamine hydrochlorideHCID 110741023-(Trifluoromethyl)phenylcyanamide

生成物 1

HCID 178512103HCID 178512103、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
150 °C

実験手順

A mixture of 3-cyanamidobenzotrifluoride (1.20 g, 6.45 mmol) and 4-chlorobenzylamine hydrochloride (1.26 g, 7.09 mmol) was stirred at 150° C. for 40 h. Dichloromethane (100 ml) was added and the mixture was washed with saturated aqueous sodium hydrogen carbonate (100 ml). The organic phase was purified by chromatography using silica gel and a mixture of methanol (10%) and dichloromethane as eluent. The product was isolated as the free base. Yield 1.05 g, 50%. M.p. 103-105° C.

後処理

  1. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate (100 ml)
  2. customThe organic phase was purified by chromatography
  3. additiona mixture of methanol (10%) and dichloromethane as eluent
  4. customThe product was isolated as the free base

出典と根拠

ORDレコード
ord-c8effcddc3a642b88b36d357be4d8d7d
出典データセット
uspto-grants-2003_05
特許番号
US06569880B2

関連ノート

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