HRID1681558

反应详情

EQUATION

反应方程式

HRID 1681558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Chloro-2-(2-chloro-4-methanesulfonylbenzoyl) -cyclohex-2-enone (1.8 g., 5 millimole) was dissolved in 50 ml of methylene chloride and stirred at room temperature. A mixture of N,N'-dimethylethylene diamine (0.22 g., 2.5 mmol mole) and triethylamine (0.5 g., 5 mml) in 10 ml of methylene chloride was added dropwise over 20 minutes and the resulting solution was stirred for 2 hours. The reaction mixture was poured into lN HCl and extracted with additional methylene chloride. The organic layer was washed with saturated NaHCO3 solution, dried with MgSO4 and the solvent evaporated to yield a yellow foam: 1.6 g., 86%. The structure is consistent with nuclear magnetic resonance, infrared and mass spectral data.

WORKUP

后处理

  1. additionwas added dropwise over 20 minutes
  2. stirringthe resulting solution was stirred for 2 hours
  3. extractionextracted with additional methylene chloride
  4. washThe organic layer was washed with saturated NaHCO3 solution
  5. dry with materialdried with MgSO4
  6. customthe solvent evaporated
  7. customto yield a yellow foam