HRID917472
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
A stirred suspension of 1.05 g (3.10 mmol) 5-iodo-2-(tetrahydro-pyran-4-yl)-pyridin-4-ylamine, 59 mg (0.31 mmol) copper(I) iodide, 112 mg (0.62 mmol) 1,10-phenanthroline and 2.02 g (6.19 mmol) cesium carbonate in 5 ml methanol was heated at 130° C. for 2×3 min in a microwave oven. The resulting mixture was then cooled to room temperature and concentrated in vacuo. Flash chromatography (methanol/dichloromethane/triethylamine) afforded 394 mg (57%) 5-methoxy-2-(tetrahydro-pyran-4-yl)-pyridin-4-ylamine as a red crystalline solid. ES-MS m/e (%): 209 (M+H+, 100).
WORKUP
后处理
- temperatureThe resulting mixture was then cooled to room temperature
- concentrationconcentrated in vacuo