反应详情

温度

0 °C

7.8 g of 2-methoxy-4-amino-5-ethylsulphonyl benzoic acid, 70 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° C. and 4.1 g of isobutyl chloroformate is poured in drop by drop. It is agitated for 45 minutes at 0° C. and 6 g of 1-cyclohexylmethyl-3-amino-pyrrolidine is dripped in. The reaction is continued for 2 hours at room temperature, 80 ml of water and 5 ml of soda lye are added, then the acetone is evaporated under vacuum. An oil is decanted; it is washed twice with 100 ml of water than dissolved hot in 50 ml ethyl acetate. It is chilled in a refrigerator. The crystals are filtered off, washed with a little ethyl acetate then dried in an oven at 50° C.

1. customfitted with an agitator
2. waitThe reaction is continued for 2 hours at room temperature
3. customthe acetone is evaporated under vacuum
4. customAn oil is decanted
5. washit is washed twice with 100 ml of water
6. dissolutionthan dissolved hot in 50 ml ethyl acetate
7. temperatureIt is chilled in a refrigerator
8. filtrationThe crystals are filtered off
9. washwashed with a little ethyl acetate
10. customthen dried in an oven at 50° C.