Hydrochloric Acid → HCID 58124940、化合物
反応式
[C:1]([N:5]([CH2:13][CH2:14][CH2:15][O:16][CH2:17][C:18]#[C:19][C:20]1[S:24][CH:23]=[N:22][CH:21]=1)[C:6](=[O:12])[C:7]([O:9]CC)=[O:8])([CH3:4])([CH3:3])[CH3:2].[OH-].[K+].Cl>O1CCOCC1.O>[C:1]([N:5]([CH2:13][CH2:14][CH2:15][O:16][CH2:17][C:18]#[C:19][C:20]1[S:24][CH:23]=[N:22][CH:21]=1)[C:6](=[O:12])[C:7]([OH:9])=[O:8])([CH3:4])([CH3:2])[CH3:3]参加物
6
反応条件
- 温度
- 55 °C
実験手順
A solution of 272 mg of 8a in 3 ml of dioxane was mixed with 170 mg of KOH in 1.5 ml of water. The mixture was stirred for 1 h at 55° C. after which all starting material had disappeared, as judged by TLC analysis. The reaction mixture was cooled, diluted with 10 ml of water and acidified to pH3 by addition of cold 0.5N HCl. The product was extracted with ethyl acetate. The combined organic layers were washed once with water, dried and concentrated. The product 8b, 210 mg, thus obtained was used without further purification in the next step.
後処理
- temperatureThe reaction mixture was cooled
- extractionThe product was extracted with ethyl acetate
- washThe combined organic layers were washed once with water
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-0e234dad5bd548be870f9b540d7703de
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08431564B2
反応ノート
読み込み中…