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ChemicalBook CAS DataBase List 3,6-Dichloro-4-methylpyridazine
19064-64-3

3,6-Dichloro-4-methylpyridazine synthesis

4synthesis methods
-

Yield:19064-64-3 89%

Reaction Conditions:

in trichlorophosphate

Steps:

1 4-methyl-3,6-dichloropyridazine
4-methyl-3,6-dichloropyridazine
A solution of 4-methyl-3,6-pyridazinediol (252 g, 2 mol) in phosphorous oxychloride (2000 ml) is refluxed on an oil bath for 7 h.
The excess amount of POCl3 is removed in vacuum, the residue is cooled and added to 5 kg of ice.
The reaction mixture is then neutralized with aqueous ammonia and extracted with chloroform (8x500 ml).
The combined organic extract is washed with brine (4x500 ml), dried over MgSO4 and the solvent is removed in vacuum, yielding the desired product (290 g, 89%).

References:

Obshchestvo S Ogranichennoy Otvetstvennostyou "Fusion Pharma";CHILOV, Germes Grigorievich;TITOV, Ilya Yurievich EP2743266, 2014, A2 Location in patent:Page/Page column

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