HRID1966618
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 Intermediate 8 (6.41 g, 16.5 mmol) in ethanol (50 mL) was added hydrazine monohydrate (12 mL, 247 mmol). The mixture was stirred at room temperature overnight, concentrated, and the residue was triturated with isopropyl alcohol. The resulting solid was filtered and the solvent removed under reduced pressure. The residue was purified by column chromatography with silica gel, eluting with methylene chloride/ethanol/ammonium hydroxide (80:8:1) to give the title compound (2.31 g, 54%) as oil.
WORKUP
后处理
- concentrationconcentrated
- customthe residue was triturated with isopropyl alcohol
- filtrationThe resulting solid was filtered
- customthe solvent removed under reduced pressure
- customThe residue was purified by column chromatography with silica gel
- washeluting with methylene chloride/ethanol/ammonium hydroxide (80:8:1)