Methanol → 1H-Perfluorohexane

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 200 cc of methanol, 74.3 g (1.1 mols) of 85% potassium hydroxide and 1 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 the dropwise addition, heating and refluxing were continued for tow hours. The conversion at that time was 98.1%. The heating and refluxing were further continued for two hours. Then, the reactor was cooled to room temperature, and 200 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 the fluorocarbon. Thus, 157 g of C6F13H having a purity of 99.1%, 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. temperatureThe heating and refluxing
8. waitwere further continued for two hours
9. dissolutionto dissolve
10. customprecipitated potassium iodide
11. customThe crude reaction solution
12. customwas separated into two layers
13. washthe fluorocarbon layer (lower layer) was further washed with 300 g of water
14. customto recover the fluorocarbon

ORDレコード

ord-21a112d1251042d38557af52c999c171

出典データセット

uspto-grants-1997_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05618986