反応式
[F:1][C:2]([F:7])([CH2:5][OH:6])[CH2:3][OH:4].C(N(CC)CC)C.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>C(Cl)Cl>[CH3:15][S:16]([O:4][CH2:3][C:2]([F:7])([F:1])[CH2:5][O:6][S:16]([CH3:15])(=[O:18])=[O:17])(=[O:18])=[O:17]参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a solution of 5 g (44.6 mmol) 2,2-difluoropropane-1,3-diol (prepared as described in J. Med. Chem. 1994, 37, 1857-1864) in DCM (50 mL) was added triethylamine (18.6 mL, 133.83 mmol) and methane sulphonyl chloride (6.9 mL, 89.22 mmol) at 0° C. and stirred for 1 h at 0° C. Thereafter the reaction mixture was quenched with water and extracted with DCM. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 2,2-difluoropropane-1,3-diyl dimethanesulfonate (9 g, 84%) which was used immediately in the next step.
後処理
- customThereafter the reaction mixture was quenched with water
- extractionextracted with DCM
- dry with materialThe organic layer was dried over anhydrous sodium sulphate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6897520d27f9497e907addb4497dad07
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09023844B2
関連ノート
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