[H-].[Na+].[F:3][CH:4]([F:7])[CH2:5][OH:6].C(Cl)Cl.Cl[C:12]1[N:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15]>O.C1COCC1>[Cl:21][C:19]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[C:12]([O:6][CH2:5][CH:4]([F:7])[F:3])[N:20]=1
NaH (55% dispersion in oil; 5.0 g, 114.6 mmol) is added portionwise at 10° C. to 2,2-difluoroethanol (6.25 mL, 99.0 mmol), DCM (200 mL) and THF (75 mL). After 10 min 2,6-dichloro-nicotinic acid (5.0 g, 24.7 mmol) is added to the reaction mixture and it is stirred at rt overnight. Then water is added and it is concentrated. The residue is diluted with water and extracted with Et2O. Formic acid is added to the aqueous layers the precipitate is filtered off, washed with water and dried to give the sub-title compound.
Loading…
