反应详情

温度

85 °C

To a suspension of (1-Carbamimidoyl-cyclopropyl)-carbamic acid tert-butyl ester (488 mg, 2.45 mmol) and K2CO3 (676 mg, 4.90 mmol) in MeCN (14 mL) at 85° C. was added a solution of 3-Bromo-1,1,1-trifluoro-propan-2-one (400 mg, 2.09 mmol) in MeCN (10 mL) drop wise over 30 min. The dilute reaction mixture (0.1 N) was stirred at 85° C. for 3 h before cooled to room temperature. Diluted with EtOAc and extracted three times, washed with water and Brine. Dried over MgSO4, filtered and concentrated down in vacuo. The mixture was purified by reverse phase preparation HPLC to give 32 mg of [1-(4-Trifluoromethyl-1H-imidazol-2-yl)-cyclopropyl]-carbamic acid tert-butyl ester as a yellow solid, m/z 292.42 [M+1]+

1. temperaturebefore cooled to room temperature
2. extractionextracted three times
3. washwashed with water and Brine
4. dry with materialDried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated down in vacuo
7. customThe mixture was purified by reverse phase preparation HPLC