Methanol → 1H-Perfluorohexane

Into a 20 l Hastelloy C autoclave equipped with a stirrer, a reflux condenser and a thermometer, 5130 g of methanol and 60 g of isopropyl alcohol and 1485 g (22.5 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 50° C. Then, 4460 g (10 mols) of C6F13I was fed thereto over a period of two hours. While maintaining the internal temperature of the reactor at a level of from 50° to 55° C., stirring was continued for 10 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 3200 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 twice with 3200 g of water to obtain 2975 g (purity: 99.9%) of C6F13H. In the reactor, no formation of tar was observed.

1. temperatureThe reactor was heated
2. customto 50° C
3. temperatureWhile maintaining the internal temperature of the reactor at a level of from 50° to 55° C.
4. waitwas continued for 10 hours
5. dissolutionto dissolve
6. customprecipitated potassium iodide
7. customThe crude reaction solution
8. customwas separated into two layers
9. washthe fluorocarbon layer (lower layer) was further washed twice with 3200 g of water

ORD record

ord-9bd192d293744168b80c0d63472273a5

Source dataset

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05557017