反应详情

In a nitrogen atmosphere, a solution of 3.9 g (0.02 mole) methyl 2-(4-hydroxyphenoxy)propanoate in 20 cc of dimethylformamide was added dropwise at about 15° C. to a suspension of 0.8 g sodium hydride in 10 cc dimethylformamide. When the evolution of hydrogen ceased, 4.7 g of (0.02 mole) 2,6,7-trichloroquinoxaline was added and the reaction mixture was heated for 5 hours at ~130° C. Filtering the reaction mixture yielded a small amount of insoluble material. The filtrate was poured into approximately 200 cc of ice-water. Sodium chloride was added to the solution which was then extracted with 1200 cc of ether (4×300). The ethereal extracts were combined and dried over magnesium sulfate. The ether was removed under vacuum and the crude product was crystallized from CH3OH. Yield 2.8 g, m.p. 100°-105°.

1. temperaturethe reaction mixture was heated for 5 hours at ~130° C
2. filtrationFiltering the reaction mixture
3. customyielded a small amount of insoluble material
4. extractionwas then extracted with 1200 cc of ether (4×300)
5. dry with materialdried over magnesium sulfate
6. customThe ether was removed under vacuum
7. customthe crude product was crystallized from CH3OH