反応式
[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:12]([CH3:29])=[C:13](/[CH:17]=[C:18]2/[C:19]3[CH:20]=[C:21]([F:28])[CH:22]=[CH:23][C:24]=3[NH:25][C:26]/2=[O:27])[NH:14][C:15]=1[CH3:16])=[O:10])[CH2:4][CH3:5].CS([O-])(=O)=O.[OH-].[Na+]>O>[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:12]([CH3:29])=[C:13](/[CH:17]=[C:18]2/[C:19]3[CH:20]=[C:21]([F:28])[CH:22]=[CH:23][C:24]=3[NH:25][C:26]/2=[O:27])[NH:14][C:15]=1[CH3:16])=[O:10])[CH2:4][CH3:5]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Sunitinib methanesulfonate (1.0 g) and H2O (60 mL) was added into a flask in r.t. and heated to 80° C., the mixture turned clear. The pH of the mixture was adjusted to 8˜9 with 1N NaOH and cooled r.t., was stirred overnight, filtered, washed, and dried in vacuo to give 0.65 g of crude sunitinib with 99.2% purity by HPLC analysis in 99.5% yield.
後処理
- temperaturecooled r.t.
- filtrationfiltered
- washwashed
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-b24cd80ef32e41859a7e5c7bd4853404
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846953B2
関連ノート
読み込み中…