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
To 1-cyclobutyl-3-(4-(piperazine-1-carbonyl)phenyl)urea (0.165 mmol, 50 mg) in tetrahydrofuran (1654 μl) was added 3-(chloromethyl)-N-(1,1,1-trifluoro-2-methylpropan-2-yl)benzamide (0.182 mmol, 50.9 mg) and triethylamine (0.496 mmol, 69.1 μl, 50.2 mg). The reaction was heated to reflux and stirred for 30 minutes then acetonitrile (0.5 mL) and sodium iodide (catalytic amount) were added. After 3 hours stirring, ethyl acetate was added and the organic mixture was washed with water and saturated sodium chloride. The organic phase was dried with sodium sulfate, filtered and concentrated under reduced pressure. This material was lyophilised to give the title compound (81 mg). MS (ESI) m/z 546.5 [M+H]+
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureto reflux
- stirringAfter 3 hours stirring
- washthe organic mixture was washed with water and saturated sodium chloride
- dry with materialThe organic phase was dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure