Sodium Carbonate → 2-Fluoro-3-(4-fluorotetrahydro-2H-pyran-4-YL)pyrazine

Temperatur

0 °C

A solution of 4-(3-fluoropyrazin-2-yl)tetrahydro-2H-pyran-4-ol (0.4 g, 2.018 mmol) in CH2Cl2 (6.73 mL) was cooled to 0° C. DAST (0.533 mL, 4.04 mmol) was added to the reaction mixture dropwise and the resulting mixture was allowed to stir at 0° C. for 2 hr. A solution of saturated sodium carbonate was added dropwise to the reaction mixture at 0° C. to quench the reaction. The heterogeneous mixture was stirred vigorously for 1 hr to ensure complete quenching. Mixture was transferred to a separatory funnel and the layers were separated after addition of more DCM and saturated bicarbonate solution. The organic layer was dried over magnesium sulfate and rotovapped to remove the volatile solvent.

1. customto quench
2. customthe reaction
3. stirringThe heterogeneous mixture was stirred vigorously for 1 hr
4. customMixture was transferred to a separatory funnel
5. customthe layers were separated
6. additionafter addition of more DCM and saturated bicarbonate solution
7. dry with materialThe organic layer was dried over magnesium sulfate
8. customto remove the volatile solvent

ORD-Eintrag

ord-dcea7773ec704679b5d4c91fa4e9dd9b

Quelldatensatz

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08053438B2