HRID1892136
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooled to room temperature
- filtrationfiltered through a pad of celite
- concentrationThe solution was concentrated under vacuum
- additionthe residue was treated with NaOH and MeOH for 2 hrs
- customThe product was purified by Prep-HPLC