反応式
[CH3:1][CH:2]1[C:6](=[O:7])[CH:5](C(OCC)=O)[C:4]2([CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)[O:3]1.[OH-].[Na+]>Cl>[CH3:1][CH:2]1[C:6](=[O:7])[CH2:5][C:4]2([CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)[O:3]1参加物
実験手順
Ethyl 2,8-dimethyl-3-oxo-1-oxa-8-azaspiro[4,5]decane-4-carboxylate (3.08 g) was dissolved in 50 ml of 1N-HCl, and the solution was heated under reflux for eight hours. The reaction mixture was allowed to cool to room temperature, then cooled in an ice-water bath, and basified by addition of 20% aqueous solution of caustic soda. This alkaline solution was extracted thrice with about 80 ml of chloroform, and the combined extract was washed with saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. Distilling off the solvent under reduced pressure from the dried solution left 2 g of yellow residue, which was purified by silica gel column chromatography by using, as eluent, a mixed solvent of chloroform/methanol (20:1 by volume), giving 1.8 g of 2,8-dimethyl-1-oxa-8-azaspiro[4,5]decan-3-one as oil. It was dissolved in ether, and ethanolic hydrogen chloride was added, thus giving its hydrochloride as crystals.
後処理
- temperaturethe solution was heated
- temperatureunder reflux for eight hours
- temperaturecooled in an ice-water bath
- extractionThis alkaline solution was extracted thrice with about 80 ml of chloroform
- extractionthe combined extract
- washwas washed with saturated aqueous solution of sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- distillationDistilling off the solvent under reduced pressure from the dried solution
- waitleft 2 g of yellow residue, which
- customwas purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-5d51820b4ad84fd091837bd637b0d5d2
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05412096
関連ノート
読み込み中…