反应详情

温度

100 °C

A 500-mL, three-neck, round-bottom flask was equipped with a mechanical stirrer, a thermocouple connected to a J-KEM temperature controller and a reflux condenser. The flask was charged with 5-bromo-6-methylpicolinohydrazonamide (100 g, 0.463 mol) and formic acid (250 mL). The resulting solution was heated to 100° C. and stirred for 48 h. Formic acid was removed under reduced pressure and the resulting slurry was treated with water (1.5 L) while vigorously stirring. The mixture was filtered and washed with water (300 mL). The solids were transferred into a round-bottom flask and treated with water (1 L) and 1 M sodium hydroxide solution until pH 7. The mixture was allowed to stir for 30 min, filtered, washed with water (300 mL) and dried in a vacuum oven at 30-35° C. for 48 h to afford the product (96 g, 92% yield) as a white solid.

1. customA 500-mL, three-neck, round-bottom flask was equipped with a mechanical stirrer
2. customFormic acid was removed under reduced pressure
3. additionthe resulting slurry was treated with water (1.5 L)
4. stirringwhile vigorously stirring
5. filtrationThe mixture was filtered
6. washwashed with water (300 mL)
7. customThe solids were transferred into a round-bottom flask
8. additiontreated with water (1 L) and 1 M sodium hydroxide solution until pH 7
9. stirringto stir for 30 min
10. filtrationfiltered
11. washwashed with water (300 mL)
12. customdried in a vacuum oven at 30-35° C. for 48 h