反应详情

温度

60 °C

A solution of Intermediate 74c (1.22 g, 3.09 mmol) in dry THF (12 mL) was treated with lithium borohydride (0.10 g, 4.64 mmol) and the mixture was stirred at 60° C. for 5 h then stood at RT overnight. The mixture was stirred at 60° C. for a further 5 h then cautiously quenched with water and diluted with EtOAc and water. The phases were separated and the aqueous layer was extracted with EtOAc (2×). The combined organic layers were washed with saturated aqueous sodium bicarbonate solution and brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by FCC, using 0-100% EtOAc in cyclohexane, to give the title compound as a colorless oil (0.68 g, 62%). LCMS (Method 3): Rt 2.89 min, m/z 375 [M+Na+].

1. waitthen stood at RT overnight
2. stirringThe mixture was stirred at 60° C. for a further 5 h
3. customthen cautiously quenched with water
4. additiondiluted with EtOAc and water
5. customThe phases were separated
6. extractionthe aqueous layer was extracted with EtOAc (2×)
7. washThe combined organic layers were washed with saturated aqueous sodium bicarbonate solution and brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. customevaporated in vacuo
11. customThe residue was purified by FCC