反应详情

温度

95 °C

A solution of 33.0 g of the above substituted acylhydrazine 1b in 132 ml of acetic acid is heated with stirring at 95° C. for 2 hours. At the end of the reaction, 65 ml of isopropyl alcohol is added to the reaction mixture. And then the whole mixture is added with stirring to 200 ml of 70° C. water. After cooling to 20° C. and stirring at that temperature for an hour, the product is collected, washed with water, dried, and recrystallized from isopropyl alcohol to give 27.2 g (47% overall from 3b or 86% from 1b) of 6-methyl3-(1-[4-nitrophenoxy]tridecyl)-7H-1, 2,4 triazolo(3,4-b)-1,3,4 -thiadiazine (4) with 95 area % by HPLC.

1. additionis added to the reaction mixture
2. additionAnd then the whole mixture is added
3. temperatureAfter cooling to 20° C.
4. stirringstirring at that temperature for an hour
5. customthe product is collected
6. washwashed with water
7. customdried
8. customrecrystallized from isopropyl alcohol