Phosphoric Acid → 4,5-Dimethyl-3-hydroxy-2,5-dihydro-2-furanone, (+)-
反応式
[Na].[O:2]=[C:3]([CH:7]([CH3:11])[CH:8]([OH:10])[CH3:9])[C:4](O)=[O:5].P(=O)(O)(O)O>O>[OH:2][C:3]1[C:4](=[O:5])[O:10][C@@H:8]([CH3:9])[C:7]=1[CH3:11]参加物
5
実験手順
840 mg of the sodium salt of compound I were dissolved in 50 ml of H2O and brought to pH 2.0 with dilute phosphoric acid. The solution was held at 85° C. for 30 minutes and, after cooling, extracted with 2×50 ml of ethyl acetate. 320 mg (yield 50%) of compound III separated after removal of the solvent. Compound III, purified by preparative thin-layer chromatography (silica gel 60), exhibited an optical rotation of: [α]D20 : 21.66° (c 1.0 in chloroform).
後処理
- temperatureafter cooling
- extractionextracted with 2×50 ml of ethyl acetate
出典と根拠
- ORDレコード
- ord-49b3bf86766d415cb1a80ab0282af004
- 出典データセット
- uspto-grants-1995_09
- 特許番号
- US05449823
反応ノート
読み込み中…