تفاعل #828713
ord-46c142f5b92c4b87ac3ca017268b5a0f
معادلة التفاعل
Cyclohexene
monochloroborane methyl sulfide
→
dicyclohexylchloroborane
المردود 80.0%
الكواشف
المذيبات
ظروف التفاعل
درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىA 250-mL round bottom flask fitted with a rubber septum, a magnetic stirring bar, and a connecting tube
- 2درجة الحرارةwas cooled in an ice bath
- 3أخرىThe solvent was removed under reduced pressure (25° C., 12 Torr)
- 4workup.DISTILLATIONDistillation
الإجراء التجريبي
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.