Potassium Hydroxide → 1H-Perfluorohexane

Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped refluxing condenser, a dropping funnel and a thermometer, 200 cc of methanol, 131 g of (1.1 mols) of 48% potassium hydroxide and 3 g of tetrabutylphosphonium bromide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 223 g (0.5 mol) of C6F13I was dropwise added thereto over a period of one hour. After completion of dropwise addition, heating and refluxing were continued for two hours. The conversion at that time was 97.0%. A fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor. The recovered liquid was washed with 300 g of water to recover the fluorocarbon. Thus, 149 g of C6F13H having a purity of 99.9%, was obtained.

1. customInto a 1 l four-necked flask equipped with a stirrer
2. distillationa distillation
3. customapparatus-equipped
4. temperaturerefluxing condenser, a dropping funnel
5. temperatureThe reactor was heated
6. customto 60° C
7. additionAfter completion of dropwise addition
8. temperatureheating
9. temperaturerefluxing
10. waitwere continued for two hours
11. distillationA fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor
12. washThe recovered liquid was washed with 300 g of water
13. customto recover the fluorocarbon

ORDレコード

ord-58ac287d8cc14b7892f4b6e9a504f375

出典データセット

uspto-grants-1997_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05618986