HRID1396817

反应详情

EQUATION

反应方程式

HRID 1396817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture of tert-butyl 3-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-6-(1-ethoxyvinyl)-3-(6-phenylpyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)-8-azabicyclo[3.2.1]octane-8-carboxylate (1.1 g, 1.3 mmol) in dioxane (7 mL) was added 4 M HCl in water (2.6 ml) at 0° C. After stirring for 10 min at 0° C., 4 M HCl in dioxane (2.6 mL) was added. The reaction mixture was stirred at 0° C. for 30 min and the cooling bath was removed to warm it up to room temperature for 15 h, at which time LC/MS analysis confirmed full consumption of starting material. The solvent was removed in vacuo to get the desired product as an HCl salt.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at 0° C. for 30 min
  2. customthe cooling bath was removed
  3. temperatureto warm it up to room temperature for 15 h
  4. customconsumption of starting material
  5. customThe solvent was removed in vacuo