反应详情

12.0 g of the neutral sulphate of N-2-aminoethyl-4-morpholinecarboxamide, 2.16 g NaOH and 100 ml of absolute ethanol were refluxed 1 h. During continuing reflux 8.6 g of 3-(4-(2-ethoxyethoxy)phenoxy-1,2-epoxypropane in 50 ml of abs. ethanol was added little by little. The resulting mixture was refluxed over night, filtered and evaporated. The residue was dissolved in 200 ml of ethyl acetate and extracted twice with water. The water phase was treated with NaCl and extracted twice with ethyl acetate. The ethyl acetate phase was dried, filtered and evaporated. The residue was crystallized from ether, and recrystallized from ethyl acetate. Yield 1.1 g. Melting point 75°-77° C. (base). The structure was determined using NMR analysis.

1. temperatureThe resulting mixture was refluxed over night
2. filtrationfiltered
3. customevaporated
4. dissolutionThe residue was dissolved in 200 ml of ethyl acetate
5. extractionextracted twice with water
6. additionThe water phase was treated with NaCl
7. extractionextracted twice with ethyl acetate
8. dry with materialThe ethyl acetate phase was dried
9. filtrationfiltered
10. customevaporated
11. customThe residue was crystallized from ether
12. customrecrystallized from ethyl acetate