HRID1927248
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 methanol (10 mL) solution of 4-benzyloxy-phenylacetic acid hydrazide (200 mg) described in Manufacturing Example 15-1 were added 2-amino-3-cyanopyridine (92 mg) and 28% sodium methoxide-methanol solution (30 mg), which was stirred for 14 hours under heating and reflux. Water and ethyl acetate were added to the reaction solution, and then the organic layer was extracted. The organic layer was washed with water and saturated brine, then dried over anhydrous magnesium sulfate and filtered, after which the filtrate was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:5) to obtain the titled compound (3 mg).
WORKUP
后处理
- temperatureunder heating
- temperaturereflux
- extractionthe organic layer was extracted
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customafter which the filtrate was evaporated under a reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:5)