Water → 1,3-Propanediol, 2,2-diethyl-, cyclic sulfite (ester)
反応式
[CH2:1]([C:3]([CH2:8][CH3:9])([CH2:6][OH:7])[CH2:4][OH:5])[CH3:2].[S:10](Cl)(Cl)=[O:11].O>C(OCC)C>[CH2:1]([C:3]1([CH2:8][CH3:9])[CH2:6][O:7][S:10](=[O:11])[O:5][CH2:4]1)[CH3:2]参加物
5
反応条件
- 温度
- 0 °C
実験手順
Step A A mixture of 2,2-diethyl-propane-1,3-diol (Aldrich) (5.5 g, 40 mmol) in anhydrous ethyl ether (100 mL) at 0° C. was added thionyl chloride (10.6 g, 90 mmol). The reaction mixture was stirred at 0° C. for 2 h. Water was added. The organic layer was separated, the aqueous layer was then extracted with ethyl ether. The combined organic layers were washed with saturated aqueous NaHCO3 solution, brine, dried over MgSO4, concentrated to give 5,5-diethyl-[1,3,2]dioxathiane 2-oxide as a colorless oil (7 g, 98%).
後処理
- customThe organic layer was separated
- extractionthe aqueous layer was then extracted with ethyl ether
- washThe combined organic layers were washed with saturated aqueous NaHCO3 solution, brine
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-469106b00cf34de2be5b9ac932a130b0
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08354444B2
反応ノート
読み込み中…