反应 #523014

ord-1fcf0d4ec13041f48604d3a8cee7ba53

反应方程式

CN
methyl amine
O=C(c1ccccc1)c1ccc(CBr)cc1
α-bromo-p-benzoyl toluene
CNCc1ccc(C(=O)c2ccccc2)cc1
4-benzoyl N-methyl benzyl amine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the solvent removed in vacuo
  2. 2
    workup.DISSOLUTIONThe resulting residue is dissolved in ether
  3. 3
    洗涤washed with water
  4. 4
    萃取The ether layer is then extracted three times with 2N hydrochloric acid
  5. 5
    workup.ADDITIONby the addition of potassium hydroxide
  6. 6
    萃取extracted with ether
  7. 7
    洗涤The ether layer is washed with water
  8. 8
    干燥dried over anhydrous magnesium sulfate
  9. 9
    其他evaporated in vacuo
  10. 10
    其他The residue is then chromatographed on silica gel

实验过程

A solution of 12.0 g. (0.379 mole) anhydrous methyl amine in 150 ml. benzene is treated dropwise with 34.8 g. (0.127 mole) α-bromo-p-benzoyl toluene in 300 ml. benzene for about 30 minutes. The resulting mixture is stirred for 4 hours at room temperature and the solvent removed in vacuo. The resulting residue is dissolved in ether and washed with water. The ether layer is then extracted three times with 2N hydrochloric acid and the acidic solution made basic by the addition of potassium hydroxide and extracted with ether. The ether layer is washed with water, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue is then chromatographed on silica gel to yield 4-benzoyl N-methyl benzyl amine (identified by spectral analysis).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04006248uspto-grants-1977_02