HRID8813

反应详情

EQUATION

反应方程式

HRID 8813 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customA 10 mL rb flask equipped with a magnetic stir bar
  2. filtrationfiltered
  3. customevaporated in vacuo
  4. customThe residue was purified on a silica gel flash chromatography column
  5. washeluted with 0–10% EtOAc-hexane
  6. customEvaporation of the purified fractions
  7. customdrying in vacuo