反应详情

温度

0 °C

To a solution of product from Step 3 (785 mg, 1.83 mmol) in THF (30 mL), cooled to 0° C. and under N2 atmosphere, there was added LiAlH4 (152 mg, 4 mmol). The resulting mixture was stirred at 0° C. for 30 minutes, then quenched carefully with ice-cold H2O, and acidified with 1N aq HCl (10 mL). The mixture was extracted twice with Et2O, and these extracts were washed 3× with brine, dried over Na2SO4, and evaporated. The residue was chromatographed, eluting with a 1:1 mixture of EtOAc and hexane, to afford the title product as a thick oil.

1. customquenched carefully with ice-cold H2O
2. extractionThe mixture was extracted twice with Et2O
3. washthese extracts were washed 3× with brine
4. dry with materialdried over Na2SO4
5. customevaporated
6. customThe residue was chromatographed
7. washeluting with a 1:1 mixture of EtOAc and hexane