反应详情

温度

107.5 °C

A mixture of N-[4-(morpholin-4-ylsulfonyl)phenyl]guanidine (85 mg, 0.3 mmol), (2E)-3-(dimethylamino)-1-[4-(trifluoromethyl)phenyl]prop-2-en-1-one (43 mg, 0.18 mmol), and potassium carbonate (83 mg, 0.6 mmol) in 1 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (DMPU) is stirred at 105 to 110° C. for 18 hrs. It is then cooled to room temperature, and diluted with water (15 ml). The resulting suspension is filtered, and the precipitate is washed with dilute citric acid and water, and then dissolved in ethyl acetate. The organic solution is passed through a pad of silica gel, and the filtrate is evaporated. The residue is triturated with a mixture of methylene chloride and hexanes to give 63 mg of a yellow solid; mp 240-241° C.; MS (ESI) m/z 465.2 (M+H); HRMS: calcd for C21H19F3N4O3S, 464.1130; found (ESI_FT), 465.11835.

1. temperatureIt is then cooled to room temperature
2. filtrationThe resulting suspension is filtered
3. washthe precipitate is washed with dilute citric acid and water
4. dissolutiondissolved in ethyl acetate
5. customthe filtrate is evaporated
6. customThe residue is triturated with a mixture of methylene chloride and hexanes