反应详情

温度

10 °C

146 g of 7-sulfamoyl-1,4-benzodioxane-5-carboxylic acid, 300 ml of dioxane and 57 g of triethylamine were introduced into a 1-liter 3-neck flask provided with an agitator, a thermometer and an introduction funnel. The mixture was heated to 40°-50° C. and 80 ml of water was added. The solution was cooled to a temperature of from 5°-10° l C. and 61.5 g of ethyl chloroformiate was added. Agitation of the mixture was maintained for one hour at 10° C. and 93 g of 1-(2-pyrimidinyl)-piperazine was added without the temperature rising above 15° C. Agitation of the mixture was continued for one hour at ambient temperature and then, after the addition of 1,500 ml of water, the mixture was rendered alkaline to a pH of 10 with ammonia. The crystals produced after distillation under vacuum of the solvents and cooling were dried off, washed with water, dried in a drying oven at 50° C. and then purified by treatment with 120 ml of chloroform. After filtration and drying, 92 g of 1-(2,3-ethylenedioxy-5-sulfamoylbenzoyl)-4-(2-pyrimidinyl)-piperazine was produced (M.P.: 239° C.; yield: 40.2%). The structure was confirmed by nuclear magnetic resonance.

1. customprovided with an agitator
2. temperatureThe mixture was heated to 40°-50° C.
3. temperatureThe solution was cooled to a temperature of from 5°-10° l C
4. additionand 61.5 g of ethyl chloroformiate was added
5. customrising above 15° C
6. customThe crystals produced
7. distillationafter distillation under vacuum of the solvents
8. temperaturecooling
9. customwere dried off
10. washwashed with water
11. customdried in a drying oven at 50° C.
12. custompurified by treatment with 120 ml of chloroform
13. filtrationAfter filtration
14. customdrying