Isopropanol → HCID 22731978、化合物
反応式
[OH-].[K+].[Cl:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[S:10][CH2:9][CH2:8][C:7]2([C:15](N)=[O:16])[OH:14].C([OH:21])(C)C>O>[Cl:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[S:10][CH2:9][CH2:8][C:7]2([C:15]([OH:16])=[O:21])[OH:14]参加物
5
実験手順
Potassium hydroxide (5.1 g, 91 mmol) and 6-chloro-4-hydroxythiochromane-4-yl-carboxamide (1.36 g, 5.58 mmol; from step (ii) above) were dissolved in water (25 mL) and isopropanol and refluxed for 2 d. The isopropanol was removed under reduced pressure and the aqueous residue was washed with diethyl ether. Acidification with aq. HCl, extraction with ethyl acetate, and then drying and concentration in vacuo afforded the sub-title compound. Yield: 0.87 g (64%).
後処理
- customThe isopropanol was removed under reduced pressure
- washthe aqueous residue was washed with diethyl ether
- extractionAcidification with aq. HCl, extraction with ethyl acetate
- customdrying
- concentrationconcentration in vacuo
出典と根拠
- ORDレコード
- ord-3d5ad0d1e80046b98e079ee8d5506cee
- 出典データセット
- uspto-grants-2004_04
- 特許番号
- US06716834B2
反応ノート
読み込み中…