反应 #828713

反应方程式

Cyclohexene

monochloroborane methyl sulfide

→

dicyclohexylchloroborane

收率 80.0%

溶剂

diethyl ether

反应条件

后处理

1. 1
   其他A 250-mL round bottom flask fitted with a rubber septum, a magnetic stirring bar, and a connecting tube
2. 2
   温度was cooled in an ice bath
3. 3
   其他The solvent was removed under reduced pressure (25° C., 12 Torr)
4. 4
   workup.DISTILLATIONDistillation

实验过程

A 250-mL round bottom flask fitted with a rubber septum, a magnetic stirring bar, and a connecting tube attached to a mercury bubbler was cooled in an ice bath and charged with diethyl ether (90 mL) under inert atmosphere. Cyclohexene (21.2 mL, 210 mmol) was added, followed by the slow addition of monochloroborane-methyl sulfide (11.6 mL, 100 mmol). The mixture was stirred at 0° C. for 2 h. The solvent was removed under reduced pressure (25° C., 12 Torr). Distillation provided pure dicyclohexylchloroborane (δ 76 ppm in hexane), 16.85 g, 80% yield, bp 104°-105° C. (0.5 mm). Synthesis of this product by this process can readily be carried out on a molar scale.

来源