反应 #40381

ord-09a95e78dab74866bdc4b0f4e523c6ac

反应方程式

CC(C)=O
acetone
Fc1ccc([CH2][Mg][Br])c(F)c1
2,4-difluorobenzylmagnesium bromide
[Cl-].[NH4+]
ammonium chloride
CC(C)(O)Cc1ccc(F)cc1F
alcohol
CC(C)(O)Cc1ccc(F)cc1F
1-(2,4-difluorophenyl)-2-methylpropan-2-ol

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度Then the mixture is refluxed for 1.5 hours
  2. 2
    其他The ether phase is separated off
  3. 3
    洗涤washed with water
  4. 4
    干燥dried with sodium sulfate
  5. 5
    其他evaporated down
  6. 6
    workup.DISTILLATIONThe fractional distillation of the residue

实验过程

11.0 mL acetone, diluted with 50 mL diethyl ether, is added dropwise to a solution of 500 mL of 0.25 molar 2,4-difluorobenzylmagnesium bromide in diethyl ether within 20 minutes. Then the mixture is refluxed for 1.5 hours and then hydrolyzed with 10% ammonium chloride solution. The ether phase is separated off, washed with water, dried with sodium sulfate, and evaporated down. The fractional distillation of the residue yields the alcohol as a colorless liquid (boiling point: 70° C.-73° C./2 mmbar). Yield: 20.0 g (86%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727984B2uspto-grants-2010_06