HRID449463

反应详情

EQUATION

反应方程式

HRID 449463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

A degassed mixture of 4-{2-[(5-bromopyridin-3-yl)acetyl]-1,2,3,4-tetrahydroisoquinolin-7-yl}-6-(4-methylpiperazin-1-yl)pyrimidin-2-amine (20 mg, 0.04 mmol), zinc cyanide (7 mg, 0.06 mmol), bis(tri-t-butylphosphine)palladium (1 mg, 0.002 mmol) and zinc (0.4 mg, 0.006 mmol) powder in anhydrous N-methylpyrrolidinone (0.1 mL, 1 mmol) was heated at 135° C. for 18 h. The mixture was adjusted to pH=10 with aqueous NH3, filtered, washed with MeOH, and purified by RP-LCMS (pH=10) to afford the desire product. Analytic LCMS (M+H)+: m/z=469.1.

WORKUP

后处理

  1. filtrationfiltered
  2. washwashed with MeOH
  3. custompurified by RP-LCMS (pH=10)
  4. customto afford the desire product