HRID877452
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A mixture of compound 44 (4 g, 14.0 mmol), ethyl 2-hydrazinylacetate (2.37 g, 15.0 mmol) and methanol (60 mL) was heated for 1.5 h. The reaction mixture was cooled to 0° C. and solvent was removed under reduced pressure. Water (100 mL) was added and the reaction mixture extracted with ethyl acetate (50 mL×3). Combined organic layer was washed with brine, dried over sodium sulphate and concentrated under reduced pressure. The crude compound was purified by column chromatography using 10% ethyl acetate in n-hexane as an eluent to afford the separated isomer 45 (1.2 g, 24%).
WORKUP
后处理
- temperaturewas heated for 1.5 h
- customsolvent was removed under reduced pressure
- additionWater (100 mL) was added
- extractionthe reaction mixture extracted with ethyl acetate (50 mL×3)
- washCombined organic layer was washed with brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated under reduced pressure
- customThe crude compound was purified by column chromatography