反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a round-bottomed flask was added (S)-4-methyl-6-((1-(1-methyl-6-(1-methyl-1H-pyrazol-5-yl)-1H-pyrrolo[3,2-b]pyridin-5-yl)ethyl)amino)-2-(methylthio)pyrimidine-5-carbonitrile (170 mg, 0.406 mmol) in acetonitrile (4616 μL) and water (4616 μL). The mixture was cooled to 0° C. and Oxone® (624 mg, 1.015 mmol) was added. The reaction mixture was stirred at 0° C. for 30 min and then allowed to warm to room temperature. After 4 hours the reaction mixture was diluted with EtOAc and washed with brine (3×). The combined organic layers were dried over Na2SO4, filtered, and concentrated to give the title compound as a yellow solid. ESI-MS m/z [M+H]+ calc'd for C21H22N8O2S, 451.16; found 451.4.
WORKUP
后处理
- temperatureto warm to room temperature
- washwashed with brine (3×)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated