Chloroacetyl chloride → N-[2-[4-(2-CHLOROACETYL)PHENYL]ETHYL]ACETAMIDE

HRID 1246448ノート

反応式

HRID 1246448 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][CH2:6][C:7](Cl)=[O:8].[C:10]1([CH2:16][CH2:17][NH:18][C:19](=[O:21])[CH3:20])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>ClCCCl>[Cl:5][CH2:6][C:7]([C:13]1[CH:14]=[CH:15][C:10]([CH2:16][CH2:17][NH:18][C:19](=[O:21])[CH3:20])=[CH:11][CH:12]=1)=[O:8]

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 70143N-(2-phenylethyl)acetamideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 2468242N-[2-[4-(2-CHLOROACETYL)PHENYL]ETHYL]ACETAMIDE収率 80.4%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒2 回

実験手順

Aluminium chloride (1.63 g) was dissolved in 1,2-dichloroethane (15 mL). Chloroacetylchloride (0. 732 mL) was added to the mixture at 0° C., and stirred additionally for 20 minutes, then N-(2-phenylethyl)acetamide (1 g) in 1,2-dichloroethane (5 mL) was added dropwise. The mixture was stirred for 1 hour at room temperature, and then poured into ice water. The mixture was extracted with chloroform, washed with water and saturated sodium chloride solution, dried over sodium sulfate and concentrated in vacuo. The solid was washed with ethyl acetate and ethyl ether, and dried in vacuo to give N-{2-[4-(2-chloroacetyl)phenyl]ethyl}acetamide as a white powder (1.18 g, 80.4%).

後処理

  1. stirringThe mixture was stirred for 1 hour at room temperature
  2. extractionThe mixture was extracted with chloroform
  3. washwashed with water and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. washThe solid was washed with ethyl acetate and ethyl ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-a403690cc2bb4df8a6938032e5213f89
出典データセット
uspto-grants-2006_10
特許番号
US07125901B2

反応ノート

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