反应详情

To a mechanically stirred suspension of 126 g of 2,2-dimethyl-1-(2-hydroxyethylidene)-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1,2,3,4-tetrahydronaphthalene in 550 ml of 2,3-dihydropyran there is added 5 ml of concentrated hydrochloric acid when under the development of heat a clear solution is being formed. After the mixture has been kept at 25° C. for one hour 400 ml of ether is added followed by an aqueous solution of potassium carbonate in water. The mixture is shaken and the organic layer is dried and evaporated, respectively. The residue is treated with petroleum ether (boiling range 40°-60° C.) which results in the formation of a clear solution covering a semi crystalline layer. From the supernatant a first crop of crystalline product can be secured. The rest can be gathered by dissolving the semi solid mass in boiling ether and cooling the ethereal solution whereupon crystallization of the product takes place. The product melts at 128°-130° C. Yield 80%.

1. temperatureof heat a clear solution
2. customis being formed
3. customthe organic layer is dried
4. customevaporated
5. additionThe residue is treated with petroleum ether (boiling range 40°-60° C.) which
6. customresults in the formation of a clear solution
7. dissolutionby dissolving the semi solid mass
8. temperaturecooling the ethereal solution
9. customwhereupon crystallization of the product