反应详情

To a solution of 2.15 g. of potassium hydroxide in 50 ml. of methanol was added 7.55 g. of 3,6-dichloro-2-methoxy benzohydroxamic acid followed by stirring until dissolution was obtained. To this solution was added dropwise 3.03 ml. methylbromoacetate in 25 ml. of methanol. The reaction mixture was refluxed for 2 hours and allowed to stir overnight at ambient temperature. To the reaction mixture was added 0.36 g. of additional potassium hydroxide and the mixture heated to reflux for 4 hours, then cooled, filtered, and the filtrate concentrated in vacuo to give a crude semi-solid product. This crude product was taken up in methylene chloride and washed with water, 5% aqueous NaHCO3, brine, then dried over MgSO4, filtered and evaporated in vacuo to give a viscuous oil. The oil crystallized from an ethyl acetate-hexane mixture to the title product as a white solid, m.p. 102°-105° C.

1. customwas obtained
2. additionTo this solution was added dropwise 3.03 ml
3. temperatureThe reaction mixture was refluxed for 2 hours
4. stirringto stir overnight at ambient temperature
5. additionTo the reaction mixture was added 0.36 g
6. temperatureto reflux for 4 hours
7. temperaturecooled
8. filtrationfiltered
9. concentrationthe filtrate concentrated in vacuo
10. customto give a crude semi-solid product
11. washwashed with water, 5% aqueous NaHCO3, brine
12. dry with materialdried over MgSO4
13. filtrationfiltered
14. customevaporated in vacuo
15. customto give a viscuous oil
16. customThe oil crystallized from an ethyl acetate-hexane mixture to the title product as a white solid, m.p. 102°-105° C.