反应详情

温度

115 °C

1-(4-hydroxyphenyl)-1,3-heptandione, 697 g, is dissolved in 2532 g acetic acid. O-(4-Nitrophenyl)hydroxylamine, 488 g, is added in portions at ca 20° C. The formed slurry is diluted with 739 g acetic acid and the mixture heated to 115° C. and stirred for 3 h. The dark solution is cooled and 1635 g water is added keeping the temperature at 70-80° C. The temperature is adjusted to 60° C. and seeding crystals are added. When crystallisation has started, the slurry is cooled to 4° C., filtered and washed with 870 g of 67% aqueous acetic acid followed by 580 g water. Drying at reduced pressure at 70° C. gives 736 g 2-butyl-3-(4-hydroxybenzoyl)-5-nitrobenzofuran. Yield 69%.

1. temperatureThe dark solution is cooled
2. customat 70-80° C
3. customis adjusted to 60° C.
4. additionseeding crystals are added
5. customWhen crystallisation
6. temperaturethe slurry is cooled to 4° C.
7. filtrationfiltered
8. washwashed with 870 g of 67% aqueous acetic acid
9. customDrying at reduced pressure at 70° C.