HRID2262996
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) and triethylamine (0.309 ml, 2.22 mmol) in tetrahydrofuran (4 ml) was added picolinoyl chloride hydrochloride (148 mg, 0.833 mmol) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was poured to water and extracted with ethyl acetate. The extract was washed with water, and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and ethyl acetate to give 53.0 mg (27.2%) of the desired product as a solid.
WORKUP
后处理
- temperaturecooling
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was recrystallized from a mixed solvent of hexane and ethyl acetate