HRID1919045
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
- 110 °C
PROCEDURE
实验过程
A 25 mL sealed tube was charged with 247b (590 mg, 1.15 mmol), 5-bromo-1-methyl-3-(2-methyl-1,2,3,4-tetrahydroisoquinolin-6-ylamino)pyrazin-2(1H)-one 221b (400 mg, 1.15 mmol), CH3COONa (189 mg, 2.3 mmol), K3PO4 (611 mg, 2.3 mmol), PdCl2(dppf) (94 mg, 0.11 mmol) suspended in CH3CN (25 mL) and water (1 mL). The mixture was heated at 110° C. for 2 hours. The mixture was evaporated and the residue was purified by silical-gel column eluting with 20:1 methylene chloride/methanol to give 247c as a brown solid (400 mg, 53%). MS: (M+H)+ 656.
WORKUP
后处理
- customA 25 mL sealed tube
- customThe mixture was evaporated
- customthe residue was purified by silical-gel column
- washeluting with 20:1 methylene chloride/methanol