PROCESS FOR THE PREPARATION OF AN AZOLE-DERIVATIVE
1. Process for the preparation of 3,3-dimethyl-1- (4-methoximinomethyl-phenoxy)-1-(1,2,4-triazol-1-yl)-butan- 2-ol of the formula (I) see diagramm : EP0248253,P7,F1 as a crystalline substance in the form of a diastereomer mixture which consists to the extent of 80% of diastereomer (A) and to the ext...
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Zusammenfassung: | 1. Process for the preparation of 3,3-dimethyl-1- (4-methoximinomethyl-phenoxy)-1-(1,2,4-triazol-1-yl)-butan- 2-ol of the formula (I) see diagramm : EP0248253,P7,F1 as a crystalline substance in the form of a diastereomer mixture which consists to the extent of 80% of diastereomer (A) and to the extent of 20% of diastereomer (B), diastereomer (A) being decisive for the fungicidal action of the compound of the formula (I), characterized in that a) 3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of the formula (II) see diagramm : EP0248253,P7,F2 is reacted with sulphuryl chloride in the presence of chlorobenzene at temperatures between 80 degrees C and 130 degrees C, b) the 1-chloro-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of the formula (III) see diagramm : EP0248253,P7,F3 produced in this reaction is then reacted with 4-hydroxybenzaldehyde oxime O-methyl ether of the formula (IV) see diagramm : EP0248253,P7,F4 in the presence of isopropanol and in the presence of potassium hydroxide or sodium hydroxide at temperatures between 40 degrees C and 90 degrees C, and c) the 3,3-dimethyl-1-(4-methoximinomethyl-phenoxy)-1- (1,2,4-triazol-1-yl)-butan-2-one of the formula (V) see diagramm : EP0248253,P7,F5 thus obtained is subsequently reduced using aluminium isopropylate in the presence of isopropanol at temperatures between 80 degrees C and 110 degrees C. |
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