反应详情

温度

70 °C

0.27 g of acetonylacetone was added to a solution of 0.5 g of α-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide (prepared as described in Example 13) dissolved in 5 ml of acetic acid, and the mixture was heated at 70° C. for 4 hours. The acetic acid used as the solvent was removed by evaporation under reduced pressure, and the residue was mixed with water to precipitate crystals. These crystals were collected by filtration, washed with water and dried. The product was purified by column chromatography through silica gel (eluent: a 98:2 by volume mixture of methylene chloride and ethanol), followed by recrystallization from ethanol to give 0.4 g of the title compound melting at 189°-190° C.

1. customwas removed by evaporation under reduced pressure
2. additionthe residue was mixed with water
3. customto precipitate crystals
4. filtrationThese crystals were collected by filtration
5. washwashed with water
6. customdried
7. customThe product was purified by column chromatography through silica gel (eluent
8. additiona 98:2 by volume mixture of methylene chloride and ethanol),
9. customfollowed by recrystallization from ethanol