HRID366280

反应详情

EQUATION

反应方程式

HRID 366280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a diethyl ether solution of isopropyl magnesium bromide, chloropentafluorobenzene is added at 0° C. to 40° C. under nitrogen with stirring in a period of thirty minutes, such that the isopropyl magnesium bromide is in 1.03 to 1.05 molar excess of the chloropentafluorobenzene. The mixture is stirred at 47° C. to 53° C.; after 5 to 10 hours, bromopentafluorobenzene is added to react with the excess isopropyl magnesium bromide, and the mixture is stirred at 25° C. for 1 hour. Any excess bromopentafluorobenzene is back-titrated in situ with isopropyl magnesium bromide to form more C6F5MgBr. The yield of C6F5MgBr is 96.1%, and 3.9% C6F5C1 remained, as determined by 19F NMR, using C6H5CF3 as a reference; no trace of iPrMgBr was seen with 1H NMR.

WORKUP

后处理

  1. stirringthe mixture is stirred at 25° C. for 1 hour