反应详情

To a solution of OBS02013 (5.5 g, 14.21 mmol) in anhydrous THF (50 mL) was added sodium borohydride (0.59 g, 15.63 mmol). The mixture was stirred at room temperature for 4 h, quenched with water (CARE!!) and filtered through a Celite pad. The filtrate was concentrated in vacuo and re-dissolved in DCM (200 mL). The organic layer was washed with brine (2×200 mL), dried (Na2SO4) and filtered. Concentration in vacuo of the combined filtrates gave OBS02015 as a pale yellow oil (5.21 g, 94%). TLC [SiO2, EtOAc-n-hexane (1:1)] Rf=0.55; 1H-NMR (270 MHz, CDCl3)=1.97 (1H, bs, OH), 3.11 (6H, s), 4.63 (2H, s), 7.55 (2H, t, J=1.5).

1. customquenched with water (CARE!!)
2. filtrationfiltered through a Celite pad
3. concentrationThe filtrate was concentrated in vacuo
4. dissolutionre-dissolved in DCM (200 mL)
5. washThe organic layer was washed with brine (2×200 mL)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationConcentration in vacuo of the combined filtrates