反应详情

温度

20 °C

0.111 g (2.772 mmol) of 2-molar aqueous sodium hydroxide solution was added to 0.200 g (0.554 mmol) of methyl[1-(6-chloropyridazin-3-yl)-5-hydroxy-3-methyl-5-phenyl-4,5-dihydro-1H-pyrazol-4-yl]acetate in 8 ml of methanol, and the mixture was stirred at 20° C. for 1 h. The methanol was removed under reduced pressure and the residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane. The aqueous phase was extracted with 15 ml of dichloromethane, acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. Drying of the combined organic phases and removal of the solvent under reduced pressure gave 0.207 g (99% of theory) of a brown wax-like solid, melting point 55° C.

1. customThe methanol was removed under reduced pressure
2. additionthe residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane
3. extractionThe aqueous phase was extracted with 15 ml of dichloromethane
4. extractionextracted three times with in each case 15 ml of dichloromethane
5. customDrying of the combined organic phases and removal of the solvent under reduced pressure
6. customgave 0.207 g (99% of theory) of a brown wax-like solid, melting point 55° C.