反应详情

8.50 g (85.1 mmol) of sodium perborate are added in portions with ice-cooling to a suspension of 13.4 g (28.4 mmol) of 6-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-yl]benzyl}-2H-pyridazin-3-one in 55 ml of THF and 55 ml of water, and the mixture is stirred at room temperature for 2 hours. The reaction mixture is filtered off through kieselguhr with suction. The filtrate is evaporated to about half of the original volume in vacuo and adjusted to a pH of 1 using 2 N hydrochloric acid. The precipitate formed is filtered off with suction, washed with water and dried in vacuo: 2-[3-(5-hydroxypyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one as pale-beige crystals; m.p. 239° C.; ESI 361.

1. filtrationThe reaction mixture is filtered off through kieselguhr with suction
2. customThe filtrate is evaporated to about half of the original volume in vacuo
3. customThe precipitate formed
4. filtrationis filtered off with suction
5. washwashed with water
6. customdried in vacuo