反应详情

温度

60 °C

A solution of 1.6 g (0.0052 mole) of 2-(4-chloro-2-fluoro-5-(2-propynyloxy)phenyl]-4-methyl-1,2,4-triazine-3.5(2H,4H)-dione (compound 21) dissolved in 5 mL of glacial acetic acid was added dropwise to a stirred suspension of 1.5 g (0.023 mole) of zinc dust in 10 mL of glacial acetic acid and 5 mL of water. After complete addition the mixture was heated at 60° C. for 1.5 hours. The mixture was filtered and the filtrate was partitioned between 50 mL of water and 50 mL of diethyl ether. The organic phase was washed first with water followed by a saturated aqueous sodium bicarbonate solution. The washed organic phase was dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated under reduced pressure to yield 1.2 g of 2-[4-chloro-2-fluoro-5-(2-propynyloxy)phenyl]-1,6-dihydro-4-methyl-1,2,4-triazine-3,5(2H,4H)-dione as an oil, compound A-3 of Table A-1.

1. additionAfter complete addition the mixture
2. filtrationThe mixture was filtered
3. customthe filtrate was partitioned between 50 mL of water and 50 mL of diethyl ether
4. washThe organic phase was washed first with water
5. dry with materialThe washed organic phase was dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customThe filtrate was evaporated under reduced pressure