Phenethylamine → 2-Chloro-N-phenethyl-acetamide

HRID 1045645

反応式

HRID 1045645 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[C:6]1([CH2:12][CH2:13][NH2:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][CH2:2][C:3]([NH:14][CH2:13][CH2:12][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4]

参加物

5

反応物 3

HCID 1001PhenethylamineHCID 6577Chloroacetyl chlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 949212-Chloro-N-phenethyl-acetamide収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Chloroacetylchloride (13.55 g, 120 mmol) was dropped into a solution of 2-phenylethylamine (12.12 g, 100 mmol), sodium bicarbonate (10.6 g, 126 mmol) in dichloromethane (100 ml) under ice cooling and the mixture was stirred for 2 hours. After addition of ice-water, the organic layer was separated and washed with 1N hydrochloric acid and brine. The solvents were removed under reduced pressure and the residue was recrystallized from mixture of water (20 ml) and methanol (30 ml) to afford 2-chloro-N-phenethyl-acetamide (18.33 g, 93%).

後処理

  1. customthe organic layer was separated
  2. washwashed with 1N hydrochloric acid and brine
  3. customThe solvents were removed under reduced pressure
  4. customthe residue was recrystallized from mixture of water (20 ml) and methanol (30 ml)

出典と根拠

ORDレコード
ord-cdd68044ea2b476f86677bb84ebdeb8d
出典データセット
uspto-grants-2013_10
特許番号
US08569294B2

関連ノート

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