反应 #40373

ord-8627ea437cdb47b29433fbbf7c6e18c6

反应方程式

[Cl-].[NH4+]
ammonium chloride
[CH3][Mg][Br]
methylmagnesium bromide
CCc1ccc(CC(C)=O)cc1
1-(4-ethylphenyl)propan-2-one
CCc1ccc(CC(C)(C)O)cc1
1-(4-ethylphenyl)-2-methylpropan-2-ol

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度while being cooled with an ice bath in such a way that the temperature
  2. 2
    其他does not exceed 30° C
  3. 3
    workup.ADDITIONAfter the addition
  4. 4
    温度the reaction mixture is refluxed for 1.5 hours
  5. 5
    其他After the removal of the organic phase
  6. 6
    萃取the aqueous phase is extracted with diethyl ether
  7. 7
    洗涤The combined ether phases are washed with water
  8. 8
    干燥dried with sodium sulfate
  9. 9
    其他evaporated down
  10. 10
    其他The oil thus obtained
  11. 11
    其他is further reacted directly

实验过程

14.8 g (90 mmol) of 1-(4-ethylphenyl)propan-2-one dissolved in diethyl ether is added dropwise to 39 mL of a 3 molar solution of methylmagnesium bromide in diethyl ether while being cooled with an ice bath in such a way that the temperature does not exceed 30° C. After the addition has ended, the reaction mixture is refluxed for 1.5 hours and then hydrolyzed with 10% ammonium chloride solution. After the removal of the organic phase, the aqueous phase is extracted with diethyl ether. The combined ether phases are washed with water, dried with sodium sulfate, and evaporated down. The oil thus obtained is further reacted directly. Yield: 15.5 g (90%).

来源

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