Reaktion #828713

ord-46c142f5b92c4b87ac3ca017268b5a0f

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05552081uspto-grants-1996_09