Water → HCID 18433843, 화합물

HRID 2305825노트

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HRID 2305825 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 18433843HCID 18433843, 화합물수율 43%

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 6344Dichloromethane용매

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온도
40 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b6638f4efac14d5f9eb8e2599337692d
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06441044B1

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