[H-].[Na+].[F:3][C:4]([F:14])([F:13])[C:5]([C:9]([F:12])([F:11])[F:10])([CH3:8])[CH2:6][OH:7].[Cl:15][C:16]1[CH:21]=[C:20](Cl)[N:19]=[CH:18][N:17]=1.[Cl-].[NH4+]>O1CCCC1>[Cl:15][C:16]1[CH:21]=[C:20]([O:7][CH2:6][C:5]([C:9]([F:11])([F:10])[F:12])([C:4]([F:13])([F:14])[F:3])[CH3:8])[N:19]=[CH:18][N:17]=1
In 4 ml of tetrahydrofuran was suspended 0.11 g of sodium hydride (60% in oil), to which 0.5 ml of a solution containing 0.44 g of 2,2-bis(trifluoromethyl)propanol in tetrahydrofuran was added dropwise at room temperature, followed by stirring for 10 minutes. To this was added dropwise 0.5 ml of a solution containing 0.3 g of 4,6-dichloropyrimidine in tetrahydrofuran at 0° C., followed by stirring at the same temperature for 1.5 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution, which was extracted three times with t-butyl methyl ether. The combined organic layers were washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate to give a crude product of 4-chloro-6-[2,2-bis(trifluoromethyl)propoxy]pyrimidine.
Wird geladen…
