HRID274937

反应详情

EQUATION

反应方程式

HRID 274937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.082 g (0.14 mmol) of the product of step C in 1.0 mL of methanol and 1.0 mL methylene chloride was added 250 gL of a 5.0 N solution of sodium hydroxide and the reaction was stirred at room temperature for 16 hours. The reaction mixture was then adjusted to pH=5-6 with dropwise addition of 6 N hydrochloric acid, and then concentrated in vacuo. The residue was redissolved in methanol, filtered, and evaporated. The mixture was then purified on a silica gel flash chromatography column eluted with CHCl3 --MeOH-NH4OH (80:15:1). Evaporation of the purified fractions and drying in vacuo afforded 0.061 g (90%) of the title compound.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was redissolved in methanol
  3. filtrationfiltered
  4. customevaporated
  5. customThe mixture was then purified on a silica gel flash chromatography column
  6. washeluted with CHCl3
  7. customEvaporation of the purified fractions
  8. customdrying in vacuo