反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureat reflux for 48 h
- temperatureThe mixture is cooled
- customthe solvent evaporated under reduced pressure
- customto afford an orange-brown solid
- customThis is partitioned between DCM (50 mL) and water (20 mL)
- customthe layers are separated
- washThe organic phase is washed with citric acid (10% aq., 3×25 mL)
- extractionThe combined washings are extracted with DCM (25 mL)
- additionmade basic by addition of NaHCO3 (s)
- extractionThe mixture is extracted with DCM (3×25 mL)
- dry with materialthe combined extracts dried over MgSO4
- customevaporated
- customThe material is used without further purification