反应详情

温度

65 °C

To a solution of 0.323 g (0.13 mmol) of the product of Step C in 10 mL of anhydrous THF was carefully added 0.1 g (2.63 mmol) of lithium aluminum hydride. The reaction mixture was then stirred overnight under a nitrogen atmosphere at 65° C. The reaction mixture was then cooled using an external ice water bath, 5.0 mL EtOAc was added. The reaction mixture was stirred an additional 20 min, at which point an excess of 2.5 N aqueous sodium hydroxide was added, followed by 50 mL EtOAc. The aqueous layer was separated and re-extracted with EtOAc. The organic layers were combined, dried (Na2SO4), filtered and evaporated in vacuo to afford the title compound.

1. temperatureThe reaction mixture was then cooled
2. additionwas added
3. customThe aqueous layer was separated
4. extractionre-extracted with EtOAc
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo