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Acetone → Meloxicam meglumine

HRID 984786
ノート
印刷プレビュー

反応式

HRID 984786 の反応式
[CH3:1][C:2]1[S:6][C:5]([NH:7][C:8]([C:10]2[N:21]([CH3:22])[S:18](=[O:20])(=[O:19])[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:11]=2[OH:23])=[O:9])=[N:4][CH:3]=1.[NH:24]([CH2:26][C@@H:27]([C@H:29]([C@@H:31]([C@@H:33]([CH2:35][OH:36])[OH:34])[OH:32])[OH:30])[OH:28])[CH3:25].CC(C)=O.C>O>[CH3:1][C:2]1[S:6][C:5]([NH:7][C:8]([C:10]2[N:21]([CH3:22])[S:18](=[O:19])(=[O:20])[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:11]=2[OH:23])=[O:9])=[N:4][CH:3]=1.[NH:24]([CH2:26][C@@H:27]([C@H:29]([C@@H:31]([C@@H:33]([CH2:35][OH:36])[OH:34])[OH:32])[OH:30])[OH:28])[CH3:25]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 180AcetoneHCID 297MethaneHCID 8567N-Methyl-D-glucamineHCID 54677470Meloxicam

生成物 1

HCID 54686397Meloxicam meglumine収率 90.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ff9de7a0846142359a729f6f7db21943
出典データセット
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06869948B1

反応ノート

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