反应详情

温度

0 °C

To a solution of 1E (2.37 g, 7.94 mmol) in THF (10 mL) and ethanol (20 mL) at 0° C. was added sodium borohydride (300 mg, 7.94 mmol) in several portions. After addition, the reaction was stirred at 0° C. for 10 min, and no starting material was detected by LC-MS. The resultant mixture was quenched with saturated aqueous NaHCO3 (30 mL) and extracted with EtOAc (3×30 mL). The combined organic layers were washed with saturated NaCl, dried (Na2SO4), filtered and concentrated. The resulting residue was purified by silica gel (120 g) column chromatography eluting with a isocratic of 15% EtOAc in hexane to give the title compound as a white solid (2.25 g, 95%). LC/MS (method A): retention time=3.06 min, (M+H)+=301.

1. additionAfter addition
2. customThe resultant mixture was quenched with saturated aqueous NaHCO3 (30 mL)
3. extractionextracted with EtOAc (3×30 mL)
4. washThe combined organic layers were washed with saturated NaCl
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe resulting residue was purified by silica gel (120 g) column chromatography
9. washeluting with a isocratic of 15% EtOAc in hexane