HRID729454

反应详情

EQUATION

反应方程式

HRID 729454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-[4-(2-bromo-5-fluorophenoxy)piperidin-1-yl]pyrazine-2-carbonitrile from Step 5 (0.200 g, 0.530 mmol) in DMF (2 mL) was added sodium azide (0.070 g, 1.06 mmol) and ammonium chloride (0.284 g, 5.30 mmol). After a period of 3 h at 130° C., the reaction mixture was cooled and partitioned between ethyl acetate and brine. The organic phase was separated, dried over sodium sulfate and evaporated. To the crude product was added a mixture of ether-hexane (1:1). The resulting solid was filtered to provide the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled
  2. custompartitioned between ethyl acetate and brine
  3. customThe organic phase was separated
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. additionTo the crude product was added
  7. additiona mixture of ether-hexane (1:1)
  8. filtrationThe resulting solid was filtered