HRID2281405

反应详情

EQUATION

反应方程式

HRID 2281405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A solution of 2-chloro-N-cyclopropyl-5-iodo-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine (200 mg, 0.409 mmol), Pd2 dba3 (23 mg, 0.025 mmol) and dppf (45 mg, 0.081 mmol) in DMF (2 mL) was degassed with Ar before being charged with Zn(CN)2 (28 mg, 0.24 mmol). The mixture was stirred at 70° C. for 2 h. Water and EtOAc were added. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was purified by a flash silica gel column, eluted with EtOAc/hexane (0-15%) to give 2-chloro-4-(cyclopropylamino)-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine-5-carbonitrile (110 mg).

WORKUP

后处理

  1. customThe organic phase was separated
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by a flash silica gel column
  5. washeluted with EtOAc/hexane (0-15%)