反应详情

To a solution of [3-(3,4-Dichloro-phenyl)-3-tetrazol-2-yl-propyl]-dimethyl-amine (2 mmol) in chloroform was added ethylchloroformate (>10 equiv.) and NaHCO3 (>20 equiv.) and this solution was refluxed for 3 h. After that, chloroform was evaporated and ethyl acetate was added and then this organic layer was washed with water 3 times. It was dried over MgSO4, filtered, evaporated and the filtrate was concentrated at reduced pressure. The residue was dissolved in ethanol and potassium hydroxide (>20 equiv.) dissolved in water was added and refluxed for 3 days. After that, ethyl acetate and sat. NaHCO3 were added and the organic layer was extracted. It was dried over MgSO4, filtered, evaporated and the filtrate was concentrated at reduced pressure. The residue was purified by column chromatography eluting with ethyl acetate and methanol: Yield 80%

1. temperaturethis solution was refluxed for 3 h
2. customAfter that, chloroform was evaporated
3. additionethyl acetate was added
4. washthis organic layer was washed with water 3 times
5. dry with materialIt was dried over MgSO4
6. filtrationfiltered
7. customevaporated
8. concentrationthe filtrate was concentrated at reduced pressure
9. dissolutionThe residue was dissolved in ethanol
10. additionwas added
11. temperaturerefluxed for 3 days
12. extractionthe organic layer was extracted
13. dry with materialIt was dried over MgSO4
14. filtrationfiltered
15. customevaporated
16. concentrationthe filtrate was concentrated at reduced pressure
17. customThe residue was purified by column chromatography
18. washeluting with ethyl acetate and methanol