HRID1892136

反应详情

EQUATION

反应方程式

HRID 1892136 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of (S)-4-(5-bromo-7-(phenylsulfonyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-N-(3-(isopropylcarbamoyl)-phenyl)-2-methylpiperazine-1-carboxamide from step D (70 mg, 0.11 mmol) in DMF (2 ml) was added Zn(CN)2 (26 mg, 0.22 mmol) and Pd(PPh3)4 (13 mg, 0.011 mmol). The mixture was heated at 150° C. for 3 min via microwave, cooled to room temperature, and filtered through a pad of celite. The solution was concentrated under vacuum, and the residue was treated with NaOH and MeOH for 2 hrs. The product was purified by Prep-HPLC to obtain (S)-4-(5-cyano-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-N-(3-(isopropylcarbamoyl)phenyl)-2-methylpiperazine-1-carboxamide as a white solid.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationfiltered through a pad of celite
  3. concentrationThe solution was concentrated under vacuum
  4. additionthe residue was treated with NaOH and MeOH for 2 hrs
  5. customThe product was purified by Prep-HPLC