HRID1471046
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
- 50 °C
PROCEDURE
实验过程
The product from Example 194C (0.595 g, 3.60 mmole) was combined in DMF (3 mL) with (1R,4R)-1,4-bis(4-nitrophenyl)butane-1,4-diyl dimethanesulfonate (0.259 g, 0.530 mmole), prepared as described in Example 37C, then heated overnight under nitrogen in an oil bath at 50° C. The reaction mixture was partitioned between ethyl acetate (50 mL) and water (50 mL). The organic phase was water washed (3×25 mL), dried over MgSO4, filtered and concentrated to an oil. Chromatography on silica gel eluting with ethyl acetate-hexane provided the title compound (0.0835 g, 34.1% yield) as an orange semi-solid.
WORKUP
后处理
- customprepared
- customThe reaction mixture was partitioned between ethyl acetate (50 mL) and water (50 mL)
- washwashed (3×25 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated to an oil