HRID2201239

反应详情

EQUATION

反应方程式

HRID 2201239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,3-Dimethyl-5-(1-methyl-1H-pyrazol-3-yl)-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (800 mg, 3.09 mmol), 4-bromo-N-methoxy-N-methylbutanamide (Intermediate P) (843 mg, 4.01 mmol) and cesium carbonate (2011 mg, 6.17 mmol) were suspended in DMF (11.100 ml) and the mixture was stirred at room temperature for 22 hours. The mixture was poured into water (50 ml) and extracted with DCM (3×100 ml). The combined organic extracts were washed with water (2×50 ml) and brine (50 ml), dried over sodium sulfate and evaporated under vacuum. Purification by mass-directed HPLC under the following conditions afforded the title compound.

WORKUP

后处理

  1. extractionextracted with DCM (3×100 ml)
  2. washThe combined organic extracts were washed with water (2×50 ml) and brine (50 ml)
  3. dry with materialdried over sodium sulfate
  4. customevaporated under vacuum
  5. customPurification by mass-directed HPLC under the following conditions