反应详情

A 15 ml aliquot of the chloroform solution of the mixed anhydride of 4-[(E)-2-(4,4-dimethyl-6-chromanyl)-2-methylvinyl]benzoic acid from Preparation 13 was added to a solution of 0.1 g (1.71 mmole) of n-propylamine in ca. 25 ml of chloroform at 0° C. The reaction mixture was filtered and then it was extracted twice with 1N hydrochloric acid. The resulting chloroform solution was dried (MgSO4) and evaporated in vacuo to give an oily solid. This solid was dissolved in diethyl ether and 2N sodium hydroxide. The layers were separated and the ether layer was filtered, dried (MgSO4) and evaporated in vacuo. The residue was recrystallized from diethyl ether-hexane, to give 0.127 g of the title compound, mp 138°-139° C.

1. filtrationThe reaction mixture was filtered
2. extractionit was extracted twice with 1N hydrochloric acid
3. dry with materialThe resulting chloroform solution was dried (MgSO4)
4. customevaporated in vacuo
5. customto give an oily solid
6. customThe layers were separated
7. filtrationthe ether layer was filtered
8. dry with materialdried (MgSO4)
9. customevaporated in vacuo
10. customThe residue was recrystallized from diethyl ether-hexane