Methanol → 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-Heptadecafluorooctane

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 250 cc of methanol and 3 g of tetrabutylphosphonium bromide and 74.3 g (1.1 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 273 g (0.5 mol) of C8F17I was dropwise added thereto over a period of one hour. After completion of the dropwise addition, heating and refluxing were continued for 8 hours. The conversion at that time was 99.6%. The reactor was cooled to room temperature. Then, 300 g of water was added to dissolve precipitated potassium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed with 300 g of water to recover a fluorocarbon. Thus, 197 g of C8F17H having a purity of 99.0%, was obtained.

1. customInto a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel
2. temperatureThe reactor was heated
3. customto 60° C
4. additionAfter completion of the dropwise addition
5. temperatureheating
6. temperaturerefluxing
7. waitwere continued for 8 hours
8. dissolutionto dissolve
9. customprecipitated potassium iodide
10. customThe crude reaction solution
11. customwas separated into two layers
12. washthe fluorocarbon layer (lower layer) was further washed with 300 g of water
13. customto recover a fluorocarbon

ORDレコード

ord-c651a9626b3742698ca1704d02ec5745

出典データセット

uspto-grants-1997_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05618986