Sodium Hydroxide → 2,3-Dihydrothieno(3,4-b)-1,4-dioxin-2-methanol
反応式
C([O:4][CH2:5][CH:6]1[O:11][C:10]2=[CH:12][S:13][CH:14]=[C:9]2[O:8][CH2:7]1)(=O)C.[OH-].[Na+]>O>[O:8]1[CH2:7][CH:6]([CH2:5][OH:4])[O:11][C:10]2=[CH:12][S:13][CH:14]=[C:9]12参加物
4
実験手順
In a 25 mL round bottom flask equipped with a reflux condenser 0.64 g (0.0030 mol) of (2,3-dihydrothieno[3,4-b][1,4]dioxin-2-yl)methyl acetate was combined with 50% NaOH in water. The reaction was refluxed overnight and then cooled to room temperature. It was then poured into an Erlenmeyer flask filled with 100 mL water. The mixture was acidified then extracted with DCM. The solvent was removed under reduced pressure and column chromatography (7:3 hexanes/ethyl acetate) was performed to give 0.46 g (90%) of product. The structure was confirmed by LC-MS and 1H/13C NMR.
後処理
- temperatureThe reaction was refluxed overnight
- additionIt was then poured into an Erlenmeyer flask
- extractionThe mixture was acidified then extracted with DCM
- customThe solvent was removed under reduced pressure and column chromatography (7:3 hexanes/ethyl acetate)
出典と根拠
- ORDレコード
- ord-fb4e4f1308a94e9fab69f96403766924
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07999121B2
反応ノート
読み込み中…