HRID1366200

反应详情

EQUATION

反应方程式

HRID 1366200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N,N-Diisopropylethylamine (360 μL, 2.2 mmol) is added to a mixture of 4-(1-isopropylpiperidin-4-yl)phenylamine (220 mg, 1.0 mmol) and 5,8-dibromoimidazo[1,2-a]pyrazine (280 mg, 1.0 mmol) in iPrOH (5 mL) and heated at reflux for 48 h. The mixture is cooled and the solvent evaporated under reduced pressure to afford an orange-brown solid. This is partitioned between DCM (50 mL) and water (20 mL) and the layers are separated. The organic phase is washed with citric acid (10% aq., 3×25 mL). The combined washings are extracted with DCM (25 mL) and then made basic by addition of NaHCO3 (s). The mixture is extracted with DCM (3×25 mL) and the combined extracts dried over MgSO4 and evaporated. The material is used without further purification.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 48 h
  3. temperatureThe mixture is cooled
  4. customthe solvent evaporated under reduced pressure
  5. customto afford an orange-brown solid
  6. customThis is partitioned between DCM (50 mL) and water (20 mL)
  7. customthe layers are separated
  8. washThe organic phase is washed with citric acid (10% aq., 3×25 mL)
  9. extractionThe combined washings are extracted with DCM (25 mL)
  10. additionmade basic by addition of NaHCO3 (s)
  11. extractionThe mixture is extracted with DCM (3×25 mL)
  12. dry with materialthe combined extracts dried over MgSO4
  13. customevaporated
  14. customThe material is used without further purification