反应详情

温度

0 °C

To a cooled (0° C.), stirred solution of 2-[3,5-dichloro-4-(3-formyl-4-methoxy-phenoxy)-phenyl]-2H-[1,2,4]triazine-3,5-dione (0.4 g) in dichloromethane (10 mL) was added 1M boron trichloride in dichloromethane (4 mL). The resulting orange slurry was stirred at ambient temperature for 5 h, ice added and the reaction stirred an additional 1 h. The two phase solution was diluted into ethyl acetate and washed with water, brine, dried (Na2SO4), concentrated in vacuo to afford the title compound of Step B as an off-white solid, 0.4 g (m.p. 146-150° C.).

1. additionice added
2. stirringthe reaction stirred an additional 1 h
3. washwashed with water, brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo