HRID1064179

反应详情

EQUATION

反应方程式

HRID 1064179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Preparation of example 168 from the title compound of Example 152 (49 mg, 0.091 mmol) and 4M HCl in dioxane (10 mL) was carried out analogously to Example 91. Isolation, also in an analogous manner, included freebasing with triethylamine and subsequent silica gel chromatography eluting with 3:1:1 hexane:ethyl acetate:ethanol. With ice bath cooling, the purified freebase in CH2Cl2 (10 mL) was treated with 4M HCl in dioxane (0.1 mL). After removal of the volatile components, the title compound (21 mg, 0.044 mmol) was obtained as an orange/yellow powder in 49% yield.

WORKUP

后处理

  1. washeluting with 3:1:1 hexane
  2. temperatureWith ice bath cooling
  3. additionthe purified freebase in CH2Cl2 (10 mL) was treated with 4M HCl in dioxane (0.1 mL)
  4. customAfter removal of the volatile components