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

Into a 500 cc four-necked equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 200 cc of methanol and 32.4 g (0.6 mol) of sodium methoxide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 273 g of (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 10 hours. The conversion at that time was 99.8%. 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 obtain 201 g of C8F17H having a purity of 99.4%. In the reactor, no formation of tar was observed.

1. customInto a 500 cc four-necked 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 10 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

ORD 기록

ord-54e288f41c9e4c46969dca265467999b

출처 데이터셋

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05557017