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ChemicalBook CAS DataBase List 3-Chloro-6-trifluoromethyl-pyridazine
258506-68-2

3-Chloro-6-trifluoromethyl-pyridazine synthesis

5synthesis methods
174607-36-4 Synthesis
6-Trifluoromethylpyridazin-3(2H)-one

174607-36-4
88 suppliers
$35.00/100mg

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Yield:258506-68-2 92%

Reaction Conditions:

with thionyl chloride;N,N-dimethyl-formamide for 2 h;Heating / reflux;

Steps:

Reference Example 313

Reference Example 313 A mixture of6- (trifluoromethyl)-3-pyridazinone (1.41 g), thionyl chloride (1.5 ml) and N, N-dimethylformamide (0.3 ml) was refluxed for 2 hours. Excess thionyl chloride was evaporated under reduced pressure and aqueous sodium hydrogen carbonate was added. The mixture was extracted with diethyl ether. The diethyl ether layer was washed with saturated brine, dried(MgS04) and concentrated. The residue was subjected to silica gel column chromatography, and 3-chloro-6- (trifluoromethyl) pyridazine (1.45 g, yield92%) was obtained as white crystals from a fraction eluted with ethyl acetate- hexane (1: 3, volume ratio). melting point:51-52 C.lH-NMR (CDC13) 6 : 7.75(1H, dd, J=8.7, 0.6 Hz), 7.82(1H, d, J=9.0Hz).

References:

WO2003/99793,2003,A1 Location in patent:Page 272

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