Diethyl Ether → HCID 178419089、化合物

温度

-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, 5 g (29.8 mmol) of pentafluorobenzene and 30 ml of diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 12.3 (29.8 mmol) of 16.1 wt. % pentane solution of tert-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. To the prepared solution of pentafluorophenyllithium was added 1 mol/L hexane solution (7.45 mL, 7.45 mmol) of boron trihalide at a temperature of -65°~-55° C., kept for 30 minutes at the same temperature with stirring and then the temperature was elevated up to the room temperature to afford a solution of lithium tetrakis(pentafluorophenyl)borate, which was subjected to quantitative determination employing pentafluorotoluene as an inner standard by means of 19FNMR. The yield was 92.3%.

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レコード

ord-54ee040f2e78487c891f24c342cb26c6

出典データセット

uspto-grants-1995_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05387727