Hexane → HCID 178419089, compound

Temperature

-65 °C

Inside of a 100 ml volume glass three-neck flask equipped with a 50 ml volume glass dropping funnel, temperature resistor and septum rubber was sufficiently replaced with nitrogen. Into the flask, 15.5 g (29.8 mmol) hexane solution of 15.5 wt. % butyllithium, 3.3 g (29.8 mmol) potassium tertbutoxide and 15 ml diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 5 g (29.8 mmol) pentafluorobenzene and 15 ml diethyl ether 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.

1. customInside of a 100 ml volume glass three-neck flask equipped with a 50 ml 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-00d91504ec0d41dcb5d1611297681646

Source dataset

uspto-grants-1995_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05387727