反应详情

To 1.58 g (0.033 moles) of 50% sodium hydride is added 15 ml DMF; then 6.3 g (0.033 moles) of 3-(4-morpholinylmethyl)phenol, dissolved in 30 ml DMB, is added dropwise to the stirred suspension at room temperature. This mixture is stirred 20 minutes and then N-(3-bromopropyl)-phthalimide, 9 g. (0.033 moles) is added to the mixture and stirred. A clear, amber solution results. After 2 hours, this solution is poured into ice-water and extracted with 100 ml of chloroform. The organic layer is washed once with 100 ml 5%NaOH, and once with 100 ml water, dried over MgSO4, filtered and evaporated. The residue is dissolved in ether and washed again with 50 ml water. Then the organic layer is dried over MgSO4, filtered and evaporated. The residue rapidly forms a white solid. This is recrystallized from acetonitrile, m.p. 90°-93° C. (yield=39 g).

1. additionis added dropwise to the stirred suspension at room temperature
2. addition(0.033 moles) is added to the mixture
3. stirringstirred
4. customA clear, amber solution results
5. waitAfter 2 hours
6. extractionextracted with 100 ml of chloroform
7. washThe organic layer is washed once with 100 ml 5%NaOH
8. dry with materialonce with 100 ml water, dried over MgSO4
9. filtrationfiltered
10. customevaporated
11. dissolutionThe residue is dissolved in ether
12. washwashed again with 50 ml water
13. dry with materialThen the organic layer is dried over MgSO4
14. filtrationfiltered
15. customevaporated
16. customThis is recrystallized from acetonitrile, m.p. 90°-93° C. (yield=39 g)