HRID1464968
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- additionthe mixture was poured onto water
- extractionthe aqueous layer was extracted with dichloromethane (twice)
- dry with materialThe combined organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography on silica gel eluting with hexane/EtOAc (1.5:1-1:1)