HRID1464968

反应详情

EQUATION

反应方程式

HRID 1464968 的结构方程式

PROCEDURE

实验过程

To a mixture of 4-isobutoxy-6-(piperazin-1-yl)pyrimidine hydrochloride (300 mg, 0.97 mmol) and triethylamine (0.68 mL, 4.9 mmol) was added chloroacetyl chloride (121 mg, 1.07 mmol) at 0° C. After being stirred at the same temperature for 30 min, the mixture was poured onto water, and the aqueous layer was extracted with dichloromethane (twice). The combined organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with hexane/EtOAc (1.5:1-1:1) to give the title compound (262 mg, 86%) as a colorless oil.

WORKUP

后处理

  1. additionthe mixture was poured onto water
  2. extractionthe aqueous layer was extracted with dichloromethane (twice)
  3. dry with materialThe combined organic layer was dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel eluting with hexane/EtOAc (1.5:1-1:1)