Reaction equation
S(Cl)(=O)(=O)[OH:2].F[C:7](F)=[CH:8][C:9]([F:12])([F:11])[F:10].[CH2:14]([OH:16])[CH3:15]>>[C:9]([CH2:8][C:7]([O:16][CH2:14][CH3:15])=[O:2])([F:12])([F:11])[F:10]Participants
4
Conditions
- Temperature
- 20 °C
Procedure
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.
Workup
- temperaturecooled in liquid nitrogen
- customevacuated
- temperatureto warm
- additionthe reaction mixture was added drop by drop into the flask
- customThe organic layer was separated
- washwashed with sodium bicarbonate, water
- customdried under MgSO4
- distillationDistillation
Sources & evidence
- ORD record
- ord-41cf697fc97a4e12acff528e5f786692
- Source dataset
- uspto-grants-2010_06
- Patent number
- US07728183B2
Linked notes
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