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3,6-DICHLORO-4-TRIFLUOROMETHYL-PYRIDAZINE synthesis

2synthesis methods
-

Yield: 76%

Reaction Conditions:

with trichlorophosphate at 120; for 1.5 h;Microwave irradiation;

Steps:

3.3
Step 3: 3,6-Dichloro-4-(trifTuoromethyl)pyridazine (C4)A solution of intermediate C3 (1.0 eq) in phosphorus oxychloride (22.0 eq) was stirred for 90 min at 1200C under MW irradiation. After completion of the reaction, solvent was evaporated under reduced pressure and the crude material purified by flash column chromatography on silica gel using 2-10% Et2θ/Petroleum ether, the desired C4 was obtained as a white solid (76% yield). 1H-NMR (400 MHz, CDCl3, 300K) δ 7.79 (IH, s).

References:

ISTITUTO DI RICERCHE DI BIOLOGIA MOLECOLARE P. ANGELETTI S.P.A. WO2009/63244, 2009, A1 Location in patent:Page/Page column 79