反应详情

温度

0 °C

7.85 g of 2,3-dimethoxy-5-sulphamoyl benzoic acid, 50 ml of acetone, 10 ml of water and 3 g of triethylamine are placed in a 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The mixture is cooled to 0° and 4.2 g of isobutyl chloroformate is poured in drop by drop. The mixture is agitated for 45 minutes at 0° C., after which 6 g of 1-cyclohexylmethyl-3-amino-pyrrolidine is dripped in. It is agitated for 2 hours at room temperature, then 80 ml of water is added and the acetone evaporated under vacuum. The product crystallises. It is filtered, washed with water then re-dissolved in 150 ml of water and 20 ml of hydrochloric acid. The solution is filtered with charcoal and the filtrate made alkaline with ammonia. An oil is precipitated and crystallises slowly. The crystals are drained, washed with water and dried in an oven at 50° C. 6.8 g (53%) of product is obtained, with a melting point of 167° C.

1. customfitted with an agitator
2. temperatureThe mixture is cooled to 0°
3. stirringIt is agitated for 2 hours at room temperature
4. customthe acetone evaporated under vacuum
5. customThe product crystallises
6. filtrationIt is filtered
7. washwashed with water
8. dissolutionthen re-dissolved in 150 ml of water
9. filtrationThe solution is filtered with charcoal
10. customAn oil is precipitated
11. customcrystallises slowly
12. washwashed with water
13. customdried in an oven at 50° C