Reacción #69620

ord-606d302f54874402afc4c8a6e2f4cb8d

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroequipped with a nitrogen feeding pipe, a reflux condenser, a dropping funnel
  2. 2
    workup.ADDITIONThe reaction mixture was treated by a conventional method
  3. 3
    Lavadothe resulting organic phase was washed with water
  4. 4
    Secadoby drying with anhydrous magnesium sulfate
  5. 5
    ConcentraciónThereafter, the resultant was concentrated under reduced pressure

Procedimiento

1.3 g of magnesium, 10.0 g of 1-bromo-4,4,4-trifluorobutane and 20 g of tetrahydrofuran were added to a four-necked flask equipped with a nitrogen feeding pipe, a reflux condenser, a dropping funnel and a thermometer, and a Grignard reagent was prepared by a conventional method. Then, a mixture containing 5.0 g of 3-pentanone and 4 g of tetrahydrofuran was dropwise added to the obtained Grignard reagent at a temperature of 25 to 35° C. over 30 minutes, followed by stirring at the same temperature for 1 hour. The reaction mixture was treated by a conventional method, and the resulting organic phase was washed with water, followed by drying with anhydrous magnesium sulfate. Thereafter, the resultant was concentrated under reduced pressure, thereby obtaining 7.9 g of 7,7,7-trifluoro-3-ethyl-3-heptanol in the form of a pale yellow oily matter.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08530598B2uspto-grants-2013_09