HRID2201229
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
- 55 °C
PROCEDURE
实验过程
Cesium carbonate (1.537 g, 4.72 mmol) was added to a solution of 1,3-dimethyl-5-(4-methylthiazol-2-yl)-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (Intermediate Nd) (0.652 g, 2.359 mmol) and 2-(3-bromo-2-(tritylthio)propyl) isoindoline-1,3-dione (2.011 g, 2.59 mmol) in dimethylacetamide (10 ml) and the mixture was stirred at 55° C. for 16 hours. The mixture was cooled to room temperature, partitioned between water (150 ml) and ethyl acetate (150 ml). The organic layer was separated, washed with brine (150 ml), dried over magnesium sulfate and evaporated under vacuum. Purification by chromatography on silica, eluting with 0-75% EtOAc/hexane afforded the title compound.
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- custompartitioned between water (150 ml) and ethyl acetate (150 ml)
- customThe organic layer was separated
- washwashed with brine (150 ml)
- dry with materialdried over magnesium sulfate
- customevaporated under vacuum
- customPurification by chromatography on silica
- washeluting with 0-75% EtOAc/hexane