HRID1014514

反应详情

EQUATION

反应方程式

HRID 1014514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-bromo-6-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)benzoic acid (1.5 g, 2.87 mmol) in THF(200 ml) was added oxalyl chloride (4.31 ml, 8.62 mmol, 2.0M DCM) and the reaction was stirred at rt for 1 hr. The reaction was concentrated on rotovap, redissolved in THF, evaporated again, and high vacced prior to next step to yield 8-bromo-5-chloro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one hydrogen chloride (1.3 g, 90%). ESIMS (M+H)+=503.

WORKUP

后处理

  1. concentrationThe reaction was concentrated on rotovap
  2. dissolutionredissolved in THF
  3. customevaporated again