Methanol → 1H-Perfluorohexane

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 256 g of methanol, 3 g of isopropyl alcohol and 46.4 g (1.16 mol) of sodium hydroxide 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 6 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 300 g of water was added to dissolve precipitated sodium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed twice with 300 g of water to obtain 145 g (purity: 99.9%) of C6F13H. In the reactor, no formation of tar was observed.

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 6 hours
8. dissolutionto dissolve
9. customprecipitated sodium iodide
10. customThe crude reaction solution
11. customwas separated into two layers
12. washthe fluorocarbon layer (lower layer) was further washed twice with 300 g of water

ORD record

ord-e3fe92d094cd49e48ba1dd0f53700ffd

Source dataset

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05557017