Water → HCID 18433843、化合物

HRID 2305825ノート

反応式

HRID 2305825 の反応式
[CH2:1]([C:3](=[CH:9][CH3:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[OH-].[Na+].[CH:13]([Cl:16])(Cl)[Cl:14].O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.ClCCl>[Cl:14][C:13]1([Cl:16])[CH:1]([CH3:2])[C:3]1([CH2:9][CH3:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5]

参加物

7

反応物 4

HCID 962WaterHCID 6212ChloroformHCID 14798Sodium HydroxideHCID 54093674Ethyl 2-ethylbut-2-enoate

生成物 1

HCID 18433843HCID 18433843、化合物収率 43%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒HCID 6344Dichloromethane溶媒

反応条件

温度
40 °C

実験手順

38 g (0.27 mol) of ethyl 2-ethylbut-2-enoate, 2.2 g (0.01 mol) of benzyltriethylammonium chloride and 57 ml of 50% strength aqueous sodium hydroxide solution were initially charged in 180 ml of dichloromethane. At 35° C. -40° C., 95 ml of chloroform were added dropwise over a period of 1 hour. After a reaction time of 5 hours at 40° C., the mixture was stirred at room temperature for a further 14 hours. For work-up, the reaction solution was poured into 1.5 l of water. The organic phase was removed and the aqueous phase was then extracted with dichloromethane. The combined organic phases were washed with water and, after drying with magnesium sulfate, concentrated. The residue (47 g) was subjected to vacuum distillation. The title compound was isolated as a colorless liquid (25.7 g, 43% yield, boiling point 71° C. at 2 mbar).

後処理

  1. customThe organic phase was removed
  2. extractionthe aqueous phase was then extracted with dichloromethane
  3. washThe combined organic phases were washed with water
  4. dry with materialafter drying with magnesium sulfate
  5. concentrationconcentrated
  6. distillationThe residue (47 g) was subjected to vacuum distillation

出典と根拠

ORDレコード
ord-b6638f4efac14d5f9eb8e2599337692d
出典データセット
uspto-grants-2002_08
特許番号
US06441044B1

反応ノート

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