Diethyl Ether → HCID 178419089, compound

Temperature

-65 °C

Inside of a 100 ml volume glass three-neck flask equipped with a 50 mol volume glass dropping funnel, temperature resistor and septum rubber was sufficiently replaced with nitrogen. Into the flask, 5 g (29.8 mmol) of pentafluorobenzene and 30 ml of diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 14.2 g (34.3 mmol) of 15.5 wt. % hexane solution of sec-butyllithium charged into the dropping funnel were added dropwise while making the inner temperature not to exceed -55° C. After the completion of dropwise addition, the reaction mixture was kept at a temperature of -65°~-55° C. with stirring to give pentafluorophenyllithium. The yield of pentafluorobenzoic acid obtained by blowing of carbon dioxide into the prepared solution of pentafluorophenyllithium was 96.8% by means of gas chromatographic quantitative determination.

1. customInside of a 100 ml volume glass three-neck flask equipped with a 50 mol volume glass
2. additionwere added dropwise
3. customto exceed -55° C
4. additionAfter the completion of dropwise addition
5. customwas kept at a temperature of -65°~-55° C.

ORD record

ord-8f23a1609568477bafe0f585c00f514d

Source dataset

uspto-grants-1995_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05387727