HRID1925501

反应详情

EQUATION

反应方程式

HRID 1925501 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 Intermediate 30 (7 g, 17.5 mmol) in dioxane (70 mL) was added hydrogen chloride (1.25M in dioxane, 25 mL). The reaction mixture was stirred at room temperature overnight. The precipitate was filtrated and washed with dioxane and ether. The crude was purified by column chromatography with silica gel, eluting with methylen chloride/methanol/ammonium (40:4:0.2) and the title compound was obtained as an oil (2.6 g, 50%). (M+): 300.

WORKUP

后处理

  1. filtrationThe precipitate was filtrated
  2. washwashed with dioxane and ether
  3. customThe crude was purified by column chromatography with silica gel
  4. washeluting with methylen chloride/methanol/ammonium (40:4:0.2)