反应详情

A mixture of 8.0 grams (0.035 moles) of 3-(4-propyl-heptyl)-morpholine, 4 grams of triethylamine, 5.8 grams (0.035 moles) of glutaric acid-monomethylesterchloride and 100 ml. of benzene were refluxed for 3 hours. After cooling the triethylamine hydrochloride formed was removed by filtration and the benzene solution was directly admixed with 12 grams of lithium aluminum hydride in 500 ml of ether. The reaction mixture was refluxed for 8 hours and decomposed by slow addition of water and sodium hydroxide. The precipitate was filtered off. The ether solution was dried and evaporated to dryness and the residue was distilled at 144°-146° C./ 0.01 mm Hg.; yield 9.8 grams (89%). The base obtained was dissolved in ether and the hydrochloride precipitated with hydrochloric acid in ethanol. After recrystallization from ethylacetate/ether, the melting point was 59°-60° C.

1. customformed
2. customwas removed by filtration
3. temperatureThe reaction mixture was refluxed for 8 hours
4. additiondecomposed by slow addition of water and sodium hydroxide
5. filtrationThe precipitate was filtered off
6. dry with materialThe ether solution was dried
7. customevaporated to dryness
8. distillationthe residue was distilled at 144°-146° C./ 0.01 mm Hg
9. customThe base obtained
10. customthe hydrochloride precipitated with hydrochloric acid in ethanol
11. customAfter recrystallization from ethylacetate/ether