Thionyl Chloride → 5,6-Dihydro-5,5-dimethyl-4H-1,3,2-dioxathiin 2-oxide
反応式
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH2:3][OH:4].[S:8](Cl)(Cl)=[O:9]>ClCCl>[CH3:1][C:2]1([CH3:7])[CH2:5][O:6][S:8](=[O:9])[O:4][CH2:3]1参加物
4
反応条件
- 温度
- 40 °C
実験手順
To a solution of 2,2-dimethyl-propane-1,3-diol (1 g) in dichloromethane (5 mL) is added dropwise at 0° C. thionylchloride (735 μL). The mixture is stirred for 3 hours at 40° C. and then partitioned between saturated aqueous NaHCO3 solution and dichloromethane. The organic phase is washed with brine and dried (MgSO4). The solvent is evaporated to give the title compound. Yield: 1 g; TLC: rf=0.65 (silicagel, cyclohexane/ethyl acetate 3:1).
後処理
- custompartitioned between saturated aqueous NaHCO3 solution and dichloromethane
- washThe organic phase is washed with brine
- dry with materialdried (MgSO4)
- customThe solvent is evaporated
出典と根拠
- ORDレコード
- ord-a87fc34e87e342288e807e1ddf50ce32
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642585B2
反応ノート
読み込み中…