Ethyl 4-chloroacetoacetate → Butanoic acid, 4-chloro-3-hydroxy-, ethyl ester

HRID 330384

반응식

HRID 330384 반응식
[Cl:1][CH2:2][C:3](=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[H][H]>C(O)C>[Cl:1][CH2:2][CH:3]([OH:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6]

참가 물질

4

반응물 2

HCID 69484Ethyl 4-chloroacetoacetateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 4377704Butanoic acid, 4-chloro-3-hydroxy-, ethyl ester수율 96.9%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

In a 200 ml-volume stainless steel-made autoclave whose atmosphere had been replaced with nitrogen were charged 8.23 g (50 mmoles) of ethyl 4-chloroacetoacetate and 20 ml of ethanol. To the mixture was added 84 mg (0.05 mmole) of Ru2Cl4 ((-)-BINAP)2 (C2H5)3N, and the mixture was heated to 100° C. When the temperature reached 100° C., 100 kg/cm2 of hydrogen was introduced into the autoclave, and the mixture was stirred under heating. After cooling to room temperature, the reaction mixture was taken out, and the ethanol was removed by distillation. Distillation of the residue gave 8.07 g (97) of ethyl 4-chloro-3-hydroxybutyrate having a boiling point of 74°-75° C./l mmHg).

후처리

  1. customreached 100° C.
  2. temperatureunder heating
  3. temperatureAfter cooling to room temperature
  4. customthe ethanol was removed by distillation
  5. distillationDistillation of the residue

출처 및 근거

ORD 기록
ord-1a18d63915d444e2a7705bff2e567dc3
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04895979

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