Phosgene → Ethyl 4-(chlorocarbonyloxy)-2-butynoate

HRID 1032565노트

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HRID 1032565 반응식
[C:1](Cl)([Cl:3])=[O:2].[OH:5][CH2:6][C:7]#[C:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]>C1C=CC=CC=1>[Cl:3][C:1]([O:5][CH2:6][C:7]#[C:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:2]

참가 물질

4

반응물 2

HCID 6371Phosgene2회HCID 108554684-Hydroxy-but-2-ynoic acid ethyl ester

생성물 1

HCID 14567687Ethyl 4-(chlorocarbonyloxy)-2-butynoate수율 85%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To 40 ml of a benzene solution of phosgene (containing 6.2 g (62.5 millimoles) of phosgene), 6.4 g (50 millimoles) of ethyl 4-hydroxy-2-butynoate was rapidly added under cooling with ice, and the mixture was stirred for 30 minutes under cooling with ice. The reaction mixture was returned to room temperature and left to stand for one night. Then, the reaction mixture was concentrated under reduced pressure to distil off benzene, whereby 8.1 g (yield: 85%) of oily ethyl 4-(chlorocarbonyloxy)-2-butynoate was obtained as the residue.

후처리

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. customwas returned to room temperature
  4. waitleft
  5. waitto stand for one night
  6. concentrationThen, the reaction mixture was concentrated under reduced pressure
  7. customto distil off benzene

출처 및 근거

ORD 기록
ord-029557b6148c4e819c563377369eb19a
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04958024

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