反应详情

To a stirred solution of 1-azido-4-chloro-2-cyclopropylbenzene (204 mg, 1.054 mmol) and methyl 3-oxobutanoate (0.341 ml, 3.16 mmol) in MeOH (2 ml) was added sodium methoxide (5M in MeOH) (1.264 ml, 6.32 mmol) dropwise and the mixture was stirred at RT for 2.5 h. The mixture was heated at 50° C. for 5 hrs and then left to stir at RT for 16 hrs. The resulting mixture was diluted with water, extracted with diethylether (×2) and the organic extracts were discarded. To the aqueous layer was added 6M HCl (aq) until acidic and this was extracted with diethyl ether. The organic extracts were dried over MgSO4, filtered and concentrated under reduced pressure to yield the title compound as an orange oil.

1. temperatureThe mixture was heated at 50° C. for 5 hrs
2. waitleft
3. stirringto stir at RT for 16 hrs
4. extractionextracted with diethylether (×2)
5. additionTo the aqueous layer was added 6M HCl (aq) until acidic and
6. extractionthis was extracted with diethyl ether
7. dry with materialThe organic extracts were dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure