HRID8813
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
A 10 mL rb flask equipped with a magnetic stir bar and a septum was charged with a solution of 50 mg (0.11 mmol) of the product of Example 90, in 2 mL MeOH, 24 mg (0.27 mmol) of manganese dioxide and ca. 5 mg of sodium cyanide was added. The reaction mixture was stirred at room temperature for 4 h, then filtered and evaporated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with 0–10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 482.2 (M+1), 484.0 (M+3); Rt=4.57 min.
WORKUP
后处理
- customA 10 mL rb flask equipped with a magnetic stir bar
- filtrationfiltered
- customevaporated in vacuo
- customThe residue was purified on a silica gel flash chromatography column
- washeluted with 0–10% EtOAc-hexane
- customEvaporation of the purified fractions
- customdrying in vacuo