反応式
[CH3:1][C@@H:2]1[C@@H:16]2[C:11](=[C:12]([OH:31])[C@:13]3([OH:30])[C:21](=[O:22])[C:20]([C:23]([NH2:25])=[O:24])=[C:19]([OH:26])[C@@H:18]([N:27]([CH3:29])[CH3:28])[C@@H:14]3[C@H:15]2[OH:17])[C:9](=[O:10])[C:8]2[C:7]([OH:32])=[CH:6][CH:5]=[CH:4][C:3]1=2.C1(C)C=CC(S([O-])(=O)=[O:40])=CC=1.[ClH:44]>CC(C)=O>[CH3:8][CH2:9][OH:10].[CH3:1][C@@H:2]1[C@@H:16]2[C:11](=[C:12]([OH:31])[C@:13]3([OH:30])[C:21](=[O:22])[C:20]([C:23]([NH2:25])=[O:24])=[C:19]([OH:26])[C@@H:18]([N:27]([CH3:28])[CH3:29])[C@@H:14]3[C@H:15]2[OH:17])[C:9](=[O:10])[C:8]2[C:7]([OH:32])=[CH:6][CH:5]=[CH:4][C:3]1=2.[OH2:40].[ClH:44]参加物
実験手順
Doxycycline p-toluenesulphonate (35.0 g) prepared as above was dissolved in a mixture of acetone (105 ml) and concentrated hydrochloric acid (16.45 ml). The solution was then filtered, and the recovered solid dried. Ethanol (35 ml) was added to the clear filtrate, and the mixture was stirred at room temperature for 2 hours 30 minutes. The crystals thus formed were filtered, washed with ethanol (41.5 ml) and then with acetone (20.75 ml), dried at 35° C. and gave 23.3 g of doxycycline hyclate. This product was indistinguishable from that obtained according to Example 4, complying in all aspects with the respective monographs in the British Pharmacopoeia 1980 and the U.S. Pharmacopoeia XX. The mother liquors were diluted with an equal volume of water and 5-sulphosalicylic acid (5.25 g) was added. After stirring overnight and recovery in the usual manner, the product, doxycycline sulphosalicylate, weighed 5.96 g.
後処理
- filtrationThe solution was then filtered
- customthe recovered solid dried
- additionEthanol (35 ml) was added to the clear filtrate
- customThe crystals thus formed
- filtrationwere filtered
- washwashed with ethanol (41.5 ml)
- dry with materialwith acetone (20.75 ml), dried at 35° C.
出典と根拠
- ORDレコード
- ord-745e20c65a33407385b81effafa89246
- 出典データセット
- uspto-grants-1986_07
- 特許番号
- US04597904
関連ノート
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