反応式
[CH:1]12[CH2:16][CH:12]([CH2:13][NH:14][CH2:15]1)[C:11]1[CH:10]=[C:9]3[C:4]([N:5]=[CH:6][CH:7]=[N:8]3)=[CH:3][C:2]2=1.[C:17]([OH:26])(=[O:25])[C@@H:18]([C@H:20]([C:22]([OH:24])=[O:23])[OH:21])[OH:19]>CO>[C:22]([C@@H:20]([C@H:18]([C:17]([O-:26])=[O:25])[OH:19])[OH:21])([O-:24])=[O:23].[CH:12]12[CH2:16][CH:1]([CH2:15][NH:14][CH2:13]1)[C:2]1[CH:3]=[C:4]3[C:9]([N:8]=[CH:7][CH:6]=[N:5]3)=[CH:10][C:11]2=1参加物
反応条件
- 温度
- 22.5 °C
実験手順
One optimized procedure for making the anhydrous Form B comprises charging a speck-free vessel with between 1.1 and 2.2 equivalents of L-tartaric add and methanol (4 to 50 volumes), and stirring this mixture until dissolved and speck-free filtering the resulting solution into a crystallization vessel. 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene free base (1.0 equivalents) and methanol (4 to 50 volumes) are stirred in a vessel until dissolved at 0 to 50° C., more preferably at 20 to 25° C. The resulting solution of 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene free base is then added over about a period of time ranging from 1 minute to 2 hours, more preferably over about 30 minutes, to the L-tartaric acid solution. The product was allowed to stir at 0 to 40° C., more preferably at 20 to 25° C., for between 1 and 48 hours, more preferably for about 1 hour, and then isolated by filtration. The product is dried generally under vacuum at 20 to 60° C., more preferably at 35 to 45° C., to give Form B of the L-tartrate salt of 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene.
後処理
- additionof L-tartaric add
- dissolutionuntil dissolved
- dissolutionuntil dissolved at 0 to 50° C., more preferably at 20 to 25° C
- customisolated by filtration
- customThe product is dried generally under vacuum at 20 to 60° C., more preferably at 35 to 45° C.
出典と根拠
- ORDレコード
- ord-761d5dc73ec54e6eb6fac0262e3e4e4f
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07265119B2
関連ノート
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