反应详情

温度

0 °C

To a cooled (0° C.), stirring solution of 2-[3-(2,4-dichloro-phenyl)-2,6-dimethyl-pyrazolo[5,1-b]oxazol-7-yloxy]-pentanoic acid ethyl ester (85 mg, 0.200 mmol) in THF (2.0 ml) at is added DIBAL-H (0.400 ml, 0.400 mmol). The reaction mixture is warmed to RT and stirred for 2 hours. The mixture is added to sat. ammonium chloride (50 ml) and the product is extracted into EtOAc (2×50 ml). The combined organics are washed with brine, dried over MgSO4 and concentrated in vacuo. The crude product is purified by ISCO combiflash chromatography, eluting with 0 to 100% (iso-hexane/EtOAc) on a 12 g SiO2-column to yield the title compound as a white solid; MS: m/z 385.13 [M+H]+.

1. temperatureThe reaction mixture is warmed to RT
2. extractionthe product is extracted into EtOAc (2×50 ml)
3. washThe combined organics are washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude product is purified by ISCO combiflash chromatography
7. washeluting with 0 to 100% (iso-hexane/EtOAc) on a 12 g SiO2-column