反応 #42131

反応方程式

ethanol

chlorosulfuric acid

1,1,3,3,3-pentafluoropropene

→

CF3CH2COOEt

収率 87.0%

反応条件

後処理

1. 1
   温度cooled in liquid nitrogen
2. 2
   その他evacuated
3. 3
   温度to warm
4. 4
   workup.ADDITIONthe reaction mixture was added drop by drop into the flask
5. 5
   その他The organic layer was separated
6. 6
   洗浄washed with sodium bicarbonate, water
7. 7
   その他dried under MgSO4
8. 8
   workup.DISTILLATIONDistillation

実験手順

A 100 mL Hastelloy shaker tube was loaded with 26.5 g (0.227 mole) chlorosulfuric acid, cooled in liquid nitrogen, evacuated and loaded with 30 g (0.225 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 40° C. at autogenous pressure for 6 hours. The pressure tube was unloaded, and the reaction mixture was added drop by drop into the flask containing 60 ml of ethanol at −10° C. over a 15 minute period. The reaction mixture was stirred overnight at 20° C. and then was poured into 200 ml of ice water. The organic layer was separated, washed with sodium bicarbonate, water, and dried under MgSO4. Distillation gave 31 g of CF3CH2COOEt (87%), bp 108-109° C.

出典