反应详情

温度

10 °C

400 ml of methylethylcetone and 11 g of methylpiperazine were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was cooled to 10° C. and then 41 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chloride were added in portions with the temperature being maintained below 20° C. After agitation of the mixture, the crystals were dried off, washed with methylethylcetone and dried and then dissolved in water and reprecipitated by addition of 50 ml of 20% ammonia. The crystals were dried off, washed with water and dried. 33 g of 5-[(4-methyl-1-piperazinyl)-carbonyl]-6,7-dibromo-8-nitro-1,4-benzodioxane were obtained (M.P.: 164° C.; yield: 69.6%).

1. customprovided with an agitator
2. temperaturebeing maintained below 20° C
3. customAfter agitation of the mixture, the crystals were dried off
4. washwashed with methylethylcetone
5. customdried
6. dissolutiondissolved in water
7. customreprecipitated by addition of 50 ml of 20% ammonia
8. customThe crystals were dried off
9. washwashed with water
10. customdried