Triethylamine → 2,2-Difluoropropane-1,3-diyl dimethanesulfonate

Temperatur

0 °C

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.

1. customThereafter the reaction mixture was quenched with water
2. extractionextracted with DCM
3. dry with materialThe organic layer was dried over anhydrous sodium sulphate
4. concentrationconcentrated

ORD-Eintrag

ord-6897520d27f9497e907addb4497dad07

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09023844B2