反应详情

温度

-70 °C

To a solution of the ester from Step 1 (3.39 g, 9.57 mmol) in toluene (75 mL) at -70° C., there was slowly added diisobutyl aluminum hydride (1M) in toluene (12 mL, 12 mmol) and the resulting mixture stirred at -70° C. for 45 minutes. Methanol (10 mL) was added slowly at -70° C., then the mixture was warmed to room temperature and water (100 mL) and 1N aqueous HCl (50 mL) were added. The mixture was shaken and the organic layer collected; the aqueous fraction was extracted with ether and the combined organic fractions washed 3 times with water, dried over MgSO4 and evaporated down to a thick oil. The crude title compound was used as such in the next step.

1. customat -70° C.
2. temperaturethe mixture was warmed to room temperature
3. stirringThe mixture was shaken
4. customthe organic layer collected
5. extractionthe aqueous fraction was extracted with ether
6. washthe combined organic fractions washed 3 times with water
7. dry with materialdried over MgSO4
8. customevaporated down to a thick oil