Ketoconazole Impurity 3 synthesis
- Product Name:Ketoconazole Impurity 3
- CAS Number:170210-49-8
- Molecular formula:C14H14Cl2N2O3
- Molecular Weight:329.18
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Yield:-
Reaction Conditions:
with potassium iodide in N,N-dimethyl acetamide;water;
Steps:
I EXAMPLE I
A mixture of 7.7 parts of 1H-imidazole, 8 parts of cis-2-(bromomethyl)-2-(2,4-dichlorophenyl)-1,3-dioxolane-4-methanol, 1 part of potassium iodide and 180 parts of N,N-dimethylacetamide is stirred and refluxed for 3 days. The reaction mixture is cooled and evaporated. Then there are added 50 parts of water and 300 parts of trichloromethane to the residue. The whole is washed three times with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 2% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 9.2 parts of cis-2-(2,4-dichlorophenyl)-2-(1H-imidazol-1-ylmethyl)-1,3-dioxolane-4-methanol; mp. 140° C.
References:
US4101665,1978,A