反应详情

温度

-78 °C

The compound of Example 13G (40 mg, 0.09 mmol) was dissolved in 1 mL of 1:1 dichloromethane/toluene and cooled to −78° C. Diisobutylaluminum hydride (1 M in hexanes, 0.36 mL) was added, and the mixture was stirred for 20 minutes. The reaction was quenched by the addition of water; the mixture was warmed to ambient temperature, and then acidified to pH˜2 by addition of concentrated HCl. The mixture was extracted with ethyl acetate; the organics were washed with brine and dried over Na2SO4. The solvents were removed in vacuo; the residue was purified by chromatography on an Analogix Intelliflash 280™, eluting with 17% ethyl acetate in hexanes to give the titled compound (25 mg, 68%).

1. customThe reaction was quenched by the addition of water
2. temperaturethe mixture was warmed to ambient temperature
3. additionacidified to pH˜2 by addition of concentrated HCl
4. extractionThe mixture was extracted with ethyl acetate
5. washthe organics were washed with brine
6. dry with materialdried over Na2SO4
7. customThe solvents were removed in vacuo
8. customthe residue was purified by chromatography on an Analogix Intelliflash 280™
9. washeluting with 17% ethyl acetate in hexanes