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

HRID 649368ノート

反応式

HRID 649368 の反応式
[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]

参加物

4

反応物 2

HCID 6371Phosgene2 回HCID 108554684-Hydroxy-but-2-ynoic acid ethyl ester

生成物 1

HCID 14567687Ethyl 4-(chlorocarbonyloxy)-2-butynoate収率 85%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94fb078edcf84d3eae5bfec031bcddbf
出典データセット
uspto-grants-1988_04
特許番号
US04739106

反応ノート

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