反应详情

tert-Butyl 3-(2-hydroxyethyl)-4-(2-(4-methyl-1-oxo-1,3-dihydroisobenzofuran-5-yl)-2-oxoethyl)piperazine-1-carboxylate (6.16 g, 14.7 mmol) was dissolved in methanol (100 mL) at 0° C. and then NaBH4 (1.67 g, 44.2 mmol) was added. The reaction mixture was warmed up to RT. After ten minutes, TLC showed no SM left. The methanol was evaporated and the residue was taken up with brine and extracted with ethyl acetate twice. The combined organic layers were dried with MgSO4, filtered and concentrated. The crude product was chromatographed through an ISCO 330 g Redi-sep column and eluted with 5% MeOH/DCM to yield the title compound: LC-MS (IE, m/z): 421[M+1]+.

1. waitAfter ten minutes
2. waitleft
3. customThe methanol was evaporated
4. extractionextracted with ethyl acetate twice
5. dry with materialThe combined organic layers were dried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was chromatographed through an ISCO 330 g Redi-sep column
9. washeluted with 5% MeOH/DCM