반응 #828713

반응 방정식

Cyclohexene

monochloroborane methyl sulfide

→

dicyclohexylchloroborane

수율 80.0%

용매

diethyl ether

반응 조건

후처리

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

실험 절차

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.

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