HRID964471

反应详情

EQUATION

反应方程式

HRID 964471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.556 g (1.50 mmol) of the product of Step B dissolved in 4.0 mL of methanol was added 0.45 mL (2.25 mmol) of a 5.0N aqueous solution of sodium hydroxide. The reaction mixture was stirred at room temperature and monitored by TLC (CHCl3 --MeOH--NH4OH 80:15:1). After 4 hours the reaction was judged to be complete and the reaction mixture was adjusted to pH=7 with 6.0N HCl. The mixture was then evaporated in vacuo and the residue was 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 0.416 g (78%) of the title compound.

WORKUP

后处理

  1. customThe mixture was then evaporated in vacuo
  2. customthe residue was purified on a silica gel flash chromatography column
  3. washeluted with CHCl3 --MeOH--NH4OH (80:15:1)
  4. customEvaporation of the purified fractions
  5. customdrying in vacuo