HRID1931779

反应详情

EQUATION

反应方程式

HRID 1931779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 4-(4,6-dimethoxy-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (1 mmol), 2 M aqueous sodium hydroxide (1 mL) and dioxane (10 mL) is heated at 40° C. for 5 h. The mixture is allowed to cool, and is then neutralized to approximately pH 7 by the addition of 1 M aqueous hydrochloric acid. Ethyl acetate and water are added. The organic layer is washed with water and brine, dried (magnesium sulfate), filtered, evaporated, and purified by flash chromatography on silica gel to give 4-(6-methoxy-4-oxo-4,5-dihydro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester.

WORKUP

后处理

  1. temperatureto cool
  2. washThe organic layer is washed with water and brine
  3. dry with materialdried (magnesium sulfate)
  4. filtrationfiltered
  5. customevaporated
  6. custompurified by flash chromatography on silica gel