HRID928823
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
- 92 °C
PROCEDURE
实验过程
A heterogeneous mixture of 2,4-dichloro-6-iodo-3-(4-(trifluoromethyl)benzyl)quinoline (515 g, 1.068 mol, Intermediate 62: step b) and sodium methoxide (577.1 g, 10.68 mol) in toluene (5.34 L) was heated to 92° C. for 18 h and then 100° C. for 13 h. After cooling to room temperature the slurry was poured over an aqueous solution of sodium bicarbonate (11.54 kg, 7 wt %, 9.615 mol). The biphasic system was mixed and then the layers were separated. The organic layer was dried over MgSO4, filtered, and concentrated to afford the title compound as a white solid.
WORKUP
后处理
- temperatureAfter cooling to room temperature the slurry
- additionThe biphasic system was mixed
- customthe layers were separated
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated