反应 #657310
ord-6897520d27f9497e907addb4497dad07
反应方程式
2,2-difluoropropane-1,3-diol
triethylamine
methane sulphonyl chloride
→
2,2-difluoropropane-1,3-diyl dimethanesulfonate
收率 84.0%
溶剂
反应条件
温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他Thereafter the reaction mixture was quenched with water
- 2萃取extracted with DCM
- 3干燥The organic layer was dried over anhydrous sodium sulphate
- 4浓缩concentrated
实验过程
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.