反応 #736550

反応方程式

phosgene

phosgene

ethyl 4-hydroxy-2-butynoate

→

ethyl 4-(chlorocarbonyloxy)-2-butynoate

収率 85.0%

溶媒

benzene

反応条件

後処理

1. 1
   温度under cooling with ice
2. 2
   温度under cooling with ice
3. 3
   その他was returned to room temperature
4. 4
   workup.WAITleft
5. 5
   workup.WAITto stand for one night
6. 6
   濃縮Then, the reaction mixture was concentrated under reduced pressure
7. 7
   その他to distil off benzene

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.

出典