HRID1878416

反应详情

EQUATION

反应方程式

HRID 1878416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureThe reaction was heated
  2. temperatureto reflux
  3. stirringAfter 3 hours stirring
  4. washthe organic mixture was washed with water and saturated sodium chloride
  5. dry with materialThe organic phase was dried with sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure