HRID624580

反应详情

EQUATION

反应方程式

HRID 624580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Cesium carbonate (115 mg, 0.351 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 Gc) (53.4 mg, 0.176 mmol) and 2-(3-bromo-2-((tert-butyldimethylsilyl)oxy)propyl)isoindoline-1,3-dione (70 mg, 0.176 mmol) in N,N-dimethylacetamide (1273 μl). The mixture was heated at 50° C. for 18 hours, then cooled to room temperature and diluted with water (30 ml). The mixture was extracted with ethyl acetate (3×30 ml), the combined organic extracts were washed with brine (90 ml), dried over sodium sulfate and evaporated under vacuum. Purification by chromatography on silica, eluting with 0-100% EtOAc/hexane, afforded the title compound.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate (3×30 ml)
  3. washthe combined organic extracts were washed with brine (90 ml)
  4. dry with materialdried over sodium sulfate
  5. customevaporated under vacuum
  6. customPurification by chromatography on silica
  7. washeluting with 0-100% EtOAc/hexane