Reaktion #737462

ord-6a4c29db4f9847e09dddbc803b75e053

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a 25 mL scintillation vial equipped with a magnetic stirrer
  2. 2
    workup.ADDITIONTo this solution was added BTSP (2.8 g, 15 mmol)
  3. 3
    SonstigeThe vial was immersed into ice/water bath
  4. 4
    SonstigeThe destruction of H2O2
  5. 5
    TrocknenThe mixture was then dried over Na2SO4
  6. 6
    EinengenConcentration

Vorschrift

In a 25 mL scintillation vial equipped with a magnetic stirrer, 1-decene (1.41 g, 10 mmol) was placed followed by addition of 4 mL dichloromethane. To this solution was added BTSP (2.8 g, 15 mmol). The vial was immersed into ice/water bath. After 5 minutes Re2O7 (24 mg, 0.05 mmol)5 was added followed by 10 μL of water. The reaction turned bright yellow and was allowed to warm up to room temperature and stirred for 14 h. Upon completion, water (3 drops) was added followed by manganese dioxide (ca. 5 mg) in order to decompose the remaining H2O2. The destruction of H2O2 was evident by the disappearance of yellow color. The mixture was then dried over Na2SO4. Concentration afforded 1-decene oxide (1.48 g, 94% yield) of a colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06271400B1uspto-grants-2001_08