Lithium Hydroxide → HCID 24958698、化合物
反応式
C([O:4][CH2:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[C:19]([C:20]#[N:21])=[C:18]([S:22][CH2:23][C:24]3[N:25]=[C:26]([C:29]4[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=4)[S:27][CH:28]=3)[N:17]=[C:16]([NH2:36])[C:15]=2[C:37]#[N:38])[CH2:10][CH2:9]1)=[O:7])(=O)C.[OH-].[Li+]>O1CCOCC1.O>[NH2:36][C:16]1[C:15]([C:37]#[N:38])=[C:14]([CH:11]2[CH2:12][CH2:13][N:8]([C:6](=[O:7])[CH2:5][OH:4])[CH2:9][CH2:10]2)[C:19]([C:20]#[N:21])=[C:18]([S:22][CH2:23][C:24]2[N:25]=[C:26]([C:29]3[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=3)[S:27][CH:28]=2)[N:17]=1参加物
5
実験手順
29 mg (0.05 mmol) of the compound from Example 25A are dissolved in a mixture of 1.5 ml of dioxane and 0.8 ml of water, and 2.4 mg (0.10 mmol) of lithium hydroxide are added. The reaction mixture is stirred at RT for two hours. After removal of the solvent on a rotary evaporator the residue is purified by preparative HPLC (column: YMC GEL ODS-AQ S-5, 15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5).
後処理
- additionare added
- customAfter removal of the solvent
- customon a rotary evaporator the residue
- customis purified by preparative HPLC (column: YMC GEL ODS-AQ S-5, 15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
出典と根拠
- ORDレコード
- ord-32c81903e6274b8a9fe9aaa4726bab27
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08304412B2
反応ノート
読み込み中…