HRID272740

反应详情

EQUATION

反应方程式

HRID 272740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of Example 516A, 1-vinyl-2-pyrrolidinone, Pd(dppf)Cl2-CH2Cl2, and triethylamine in DMF was heated at 110° C. overnight, cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered and concentrated. The concentrate was purified by column chromatography on silica gel using a solvent gradient that increased from 1 to 4% methanol in dichloromethane to give the title compound. MS (ESI) m/e 384 (M+H)+.

WORKUP

后处理

  1. washwashed with water and brine
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe concentrate was purified by column chromatography on silica gel using a solvent gradient that
  6. temperatureincreased from 1 to 4% methanol in dichloromethane