Chloroacetyl chloride → N-(3-allyloxy-2-hydroxypropyl)-N-n-propyl-alpha-chloroacetamide

HRID 1283103ノート

反応式

HRID 1283103 の反応式
[CH2:1]([O:4][CH2:5][CH:6]([OH:12])[CH2:7][NH:8][CH2:9][CH2:10][CH3:11])[CH:2]=[CH2:3].C(N(CC)CC)C.[Cl:20][CH2:21][C:22](Cl)=[O:23]>C(Cl)Cl>[CH2:1]([O:4][CH2:5][CH:6]([OH:12])[CH2:7][N:8]([CH2:9][CH2:10][CH3:11])[C:22](=[O:23])[CH2:21][Cl:20])[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 214303991-Allyloxy-3-n-propylamino-2-propanol

生成物 1

HCID 21519217N-(3-allyloxy-2-hydroxypropyl)-N-n-propyl-alpha-chloroacetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 1-allyloxy-3-n-propylamino-2-propanol (95.2 g.) in a mixture of dry methylene chloride (275 ml.), and triethylamine (80 ml.) is cooled to between -5°C. and 0°C. and a solution of chloroacetylchloride (42 ml.) in methylene chloride (60 ml.) is added dropwise with stirring during 2 hours. The mixture is allowed to warm to ambient temperature (18°-20°C.) and stirred at this temperature for 18 hours. The solution is washed with 2N hydrochloric acid (2 × 100 ml.) and then with water (100 ml.) and dried (MgSO4). Removal of the solvent under reduced pressure gives N-(3-allyloxy-2-hydroxypropyl)-N-n-propyl-α-chloroacetamide (119.7 g.) as an oil which is used without further purification.

後処理

  1. temperatureis cooled to between -5°C. and 0°C.
  2. stirringstirred at this temperature for 18 hours
  3. washThe solution is washed with 2N hydrochloric acid (2 × 100 ml.)
  4. dry with materialwith water (100 ml.) and dried (MgSO4)
  5. customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-e297cbd5871b41769297557402abfcc6
出典データセット
uspto-grants-1976_08
特許番号
US03974158

反応ノート

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