反应详情

To a suspension of 0.70 g (18.4 mmol) of LiAlH4 in 60 mL of THF, 2.25 g (5.84 mmol) of 39 was added. This reaction mixture was refluxed for 2 hr, and then saturated aqueous Na2SO4 was added. The organic layer was separated, and the aqueous layer was extracted with 2×50 mL of diethyl ether. The combined organic extract was evaporated to dryness, and the product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: hexanes-diethyl ether from 100:1 to 20:1, vol.) to yield 1.45 g (64%) of Fl.

1. additionwas added
2. temperatureThis reaction mixture was refluxed for 2 hr
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with 2×50 mL of diethyl ether
5. extractionThe combined organic extract
6. customwas evaporated to dryness
7. customthe product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: hexanes-diethyl ether from 100:1 to 20:1, vol.)
8. customto yield 1.45 g (64%) of Fl