HRID530298

反应详情

EQUATION

反应方程式

HRID 530298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of 3-(1H-pyrazol-3-yl)pyridine (0.435 g, 3 mmol) in tetrahydrofuran (15 ml) was added pyridine (0.367 ml, 4.50 mmol), DMAP (18.33 mg, 0.150 mmol). The solution was treated with 4-morpholinecarbonyl chloride (0.368 ml, 3.15 mmol). The reaction was heated to 80° C. for 20 hours. THF was removed by vacuum, the residue was partitioned between DCM and water. The organic phase was dried over MgSO4 and filtered. After evaporation the crude product was chromatographed in petroleumether:EtOAc=2:1. (Yield: 174 mg, 21%).

WORKUP

后处理

  1. customTHF was removed by vacuum
  2. customthe residue was partitioned between DCM and water
  3. dry with materialThe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. customAfter evaporation the crude product
  6. customwas chromatographed in petroleumether