反应详情

温度

20 °C

12.5 kg (35.57 mol) meloxicam and 6.9 kg (35.57 mol) meglumin are added successively, with stirring, to a mixture of 275 1 of acetone and 7:1 of water in a suitable reactor 1, then 1 kg of industrial-grade activated charcoal are added. The reaction mixture is heated and refluxed for 30 minutes. Then the mixture is forced through a pressure filter into a second reactor II. Reactor I and the pressure filter are washed out with 101 of acetone. The mixture is combined with 10-15 g meloxicam meglumin salt monohydrate seed crystals, cooled to 20° C. and stirred for 2 hours at this temperature. Then the mixture is heated, refluxed for 15 minutes and then slowly cooled to 20° C., during which time a fine crystalline crystal suspension is formed. This is stirred for 15 hours at 20° C. The crystal suspension is then centrifuged and subsequently spun dry. The centrifugal pellet is washed with 351 of acetone and again spun dry. The product is dried in the drying cupboard at 20-35° C. with fresh air for about 24 hours. Yield: 90.1% of theory; pale yellow crystalline powder, needle-like crystals; melting point: 120° C.

1. additionare added
2. temperatureThe reaction mixture is heated
3. temperaturerefluxed for 30 minutes
4. filtrationfilter into a second reactor II
5. filtrationReactor I and the pressure filter
6. washare washed out with 101 of acetone
7. temperatureThen the mixture is heated
8. temperaturerefluxed for 15 minutes
9. temperatureslowly cooled to 20° C., during which time a fine crystalline crystal suspension
10. customis formed
11. stirringThis is stirred for 15 hours at 20° C
12. customcentrifuged and subsequently spun dry
13. washThe centrifugal pellet is washed with 351 of acetone
14. customagain spun dry
15. customThe product is dried in the drying cupboard at 20-35° C. with fresh air for about 24 hours