Reacción #589101

ord-e9984706c97648daa4d4da5956ff6f64

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONcarefully added
  2. 2
    OtroAfter separation
  3. 3
    Secadothe organic layer was dried over magnesium sulphate
  4. 4
    Otroevaporated under reduced pressure
  5. 5
    workup.DISTILLATIONThe crude product was distilled under high vacuum
  6. 6
    Otroto afford

Procedimiento

A mixture (400 mL) of diethyl oxide:water 1:1 was cooled at 0° C. under nitrogen in a three-necked flask of 1 L. Sodium borohydride (3 g, 79.4 mmol) and then tricyclohexyltin hydroxide (30 g, 62.2 mmol) were successively and carefully added. After addition of 100 mL of diethyl oxide, the mixture was stirred 2 days at room temperature. After separation, the organic layer was dried over magnesium sulphate and evaporated under reduced pressure. The crude product was distilled under high vacuum to afford, a colourless oil (23.23 g; 63 mmol).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07772417B2uspto-grants-2010_08