反应详情

温度

50 °C

To a 25 mL volume three-necked flask, 1.0 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(2-methyl-1-propylidene)hydrazine ((40-b)-(15)-4), 3.8 ml of methanol and 330 mg of 50 wt % hydroxylamine aqueous solution were added, and the mixture was stirred at 50° C. for 2.5 hours and then 60° C. for 14.5 hours. The reaction mixture was concentrated under reduced pressure and water and t-butyl methyl ether were added to the residue. The precipitated crystals were collected by filtration, washed with hexane and dried to give 0.63 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methylhydrazine ((12-2)-(11)-39).

1. wait60° C. for 14.5 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure and water and t-butyl methyl ether
3. additionwere added to the residue
4. filtrationThe precipitated crystals were collected by filtration
5. washwashed with hexane
6. customdried