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US 2003/0153790 A1Published application
Process for the preparation of 1-(2,6,6-trimethyl-2-cyclohexene-1-yl)-but-2-ene-1-one
OwnerKudli Shrinivas Prashanth Kumar, Nagaraj Surekhainventors
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Abstract
The present invention relates to a novel process for the preparation of 1-(2,6,6-trimethyl-2-cyclohexene-1-yl)-2-but-2-ene-1-one commonly known as α-Damascone, by acylation of unsaturated cyclic hydrocarbon 2,6,6-trimethyl-1-cyclohexene followed by work up and its purification by vacuum distillation. 1
Claims11
A process for the preparation of α-Damascone [1-(2,6,6-trimethyl-2-cyclohexene-1-yl)-2-buten-1-one] represented by formula (II)
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- said process comprising the steps of:
- (a) adding 2,6,6-trimethyl-1-cyclohexene over a period of 30-95 minutes to a refluxing mixture of an hydrocarbon solvent, Lewis acid and Crotonic anhydride at a temperature in the range of 60-120° C.;
- (b) cooling the reaction mixture of step (a) to an ambient temperature of 25-30° C.;
- (c) pouring the cooled reaction mixture of step (b) into aqueous alkali carbonate solution and stirring the reaction mixture for about 5-20 minutes;
- (d) separating the organic layer and washing the organic layer of step (c) with water till the washing becomes neutral;
- (e) drying and removing organic solvent from the organic layer to obtain crude product and purifying the crude product to obtain pure α-Damascone of formula (II).
4 more elements
Dependencies are inferred from the claim text.