反应详情

温度

-78 °C

The compound of Example 18B (130 mg, 0.3 mmol) was dissolved in 1 mL of 1:1 dichloromethane/toluene and cooled to −78° C. Diisobutylaluminum hydride (1 M in hexanes, 0.7 mL, 2.5 equivalents) was added, and the mixture was stirred for 30 minutes. Reaction was quenched by the addition of methanol, followed by saturated aqueous NH4Cl; the mixture was warmed to ambient temperature and 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 15% ethyl acetate in hexanes, to give the titled compound (111 mg, 95%).

1. customReaction
2. customwas quenched by the addition of methanol
3. temperaturethe mixture was warmed to ambient temperature
4. extractionextracted 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 15% ethyl acetate in hexanes