تفاعل #657310
ord-6897520d27f9497e907addb4497dad07
معادلة التفاعل
2,2-difluoropropane-1,3-diol
triethylamine
methane sulphonyl chloride
→
2,2-difluoropropane-1,3-diyl dimethanesulfonate
المردود 84.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىThereafter the reaction mixture was quenched with water
- 2استخلاصextracted with DCM
- 3تجفيفThe organic layer was dried over anhydrous sodium sulphate
- 4تركيزconcentrated
الإجراء التجريبي
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.