HRID77409

反应详情

EQUATION

反应方程式

HRID 77409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 6-bromo-3-methylthieno[2,3-d]pyrimidin-4(3H)-one (70 mg, 0.28 mmol), copper(I) iodide (13.6 mg, 0.071 mmol), L-proline (16.4 mg, 0.143 mmol), 1,4-diazabicyclo[3.2.2]nonane (54.1 mg, 0.428 mmol) and potassium phosphate (132 mg, 0.571 mmol) in DMSO (1 mL) was heated at 90° C. in a sealed vessel for 3 days. The reaction was acidified with acetic acid, diluted with methanol and purified on a scx cartridge (1 g), further purified by acid prep HPLC, passed through a scx cartridge (500 mg) and evaporated to dryness to afford 6-(1,4-Diazabicyclo[3.2.2]nonan-4-yl)-3-methylthieno[2,3-d]pyrimidin-4(3H)-one (1.8 mg, 0.006 mmol).

WORKUP

后处理

  1. custompurified on a scx cartridge (1 g)
  2. customfurther purified by acid prep HPLC
  3. customevaporated to dryness