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 mixture of (2,4-dichloro-8-methyl-3-(3-(trifluoromethyl)benzyl)quinolin-6-yl)(1-methyl-1H-imidazol-5-yl)methanone (0.87 g, 1.83 mmol, Intermediate 15: step c) and dry sodium methoxide (0.58 g, 10.75 mmol) in toluene was heated in a sealed tube at 110° C. for 12 hours. Starting material was still present, therefore additional NaOCH3 (198 mg, 3.66 mmol) was added and stirring was continued at 110° C. for another 24 hours. The mixture was then cooled to room temperature, diluted with DCM, stirred at room temperature for 30 minutes, and the resulting suspension filtered through Celite®, rinsing several times with DCM. The solvents were removed under reduced pressure and the white solid product was precipitated from MeOH, filtered and dried to provide the title compound.
WORKUP
后处理
- temperatureThe mixture was then cooled to room temperature
- stirringstirred at room temperature for 30 minutes
- filtrationthe resulting suspension filtered through Celite®
- washrinsing several times with DCM
- customThe solvents were removed under reduced pressure
- customthe white solid product was precipitated from MeOH
- filtrationfiltered
- customdried