反应详情

温度

120 °C

A mixture of [5-chloro-6-oxo-1-(tetrahydro-pyran-2-yl)-1,6-dihydro-pyridazin-4-yl]-(2-trifluoromethyl-phenyl)-acetonitrile (550 mg, 1.38 mmol) in concentrated hydrochloric acid (8.4 mL), glacial acetic acid (2.1 mL) and water (2.1 mL) (4:1:1, 0.11 M) was heated to 120° C. overnight. After this time, the reaction was cooled to 25° C. and then poured onto ice, followed by rinsing with minimal water. The resulting aqueous mixture was brought to pH=4-5 by treatment with a 4N aqueous sodium hydroxide solution. The resulting tan solids were collected by filtration. The solids were subsequently washed with water (2×10 mL) and dried in vacuo to afford 4-chloro-5-(2-trifluoromethyl-benzyl)-2H-pyridazin-3-one (0.24 g, 62%) as a tan solid; ES+-HRMS m/e calcd for C12H8N2OF3Cl [M+H+] 289.0350, found 289.0350.

1. temperatureAfter this time, the reaction was cooled to 25° C.
2. additionpoured onto ice
3. washby rinsing with minimal water
4. filtrationThe resulting tan solids were collected by filtration
5. washThe solids were subsequently washed with water (2×10 mL)
6. customdried in vacuo