反应详情

温度

21 °C

To a stirred solution of 4-{4-[7-(4-cyano-3-trifluoromethylphenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]oct-5-yl]-phenyl}-butyric acid methyl ester (67) [ND-4] (61 mg, 0.12 mmol) in dichloromethane (5 mL), 1M diisobutylaluminum hydride (DIBAL) solution in hexane (0.16 mL, 0.16 mmol) was added at −78° C. After 30 min, the reaction mixture was quenched with saturated Rochelle's salt solution. The resulting mixture was stirred at 21° C. until both phases were clearly separated and the organic layer was clear. After extraction, the separated organic layer was dried over MgSO4, filtered, and concentrated under vacuum. The crude mixture of (66) and (68) was purified by flash column chromatography (hexane:ethyl acetate,

1. customthe reaction mixture was quenched with saturated Rochelle's salt solution
2. customwere clearly separated
3. extractionAfter extraction
4. dry with materialthe separated organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. additionThe crude mixture of (66) and (68)
8. customwas purified by flash column chromatography (hexane