反应详情

To a stirred solution of dimethyl 2-methyl-2-(4-nitrophenyl)malonate (5 g, 18.72 mmol, 1.0 eq) in methanol (50 mL) was added NaBH4 (2.12 g, 56.17 mmol, 3.0 eq) at 0° C. and stirred at RT for 16 h. The solvent was evaporated and the residue was diluted with water (50 mL). The product was extracted with EtOAc (2×60 mL). The combined organic layer was washed with brine (20 mL), dried over anhydrous Na2SO4, evaporated under reduced pressure. The crude product obtained was purified by CC using EtOAc/PE (1:1) to get 2-methyl-2-(4-nitrophenyl)propane-1,3-diol (1.6 g 40%; TLC system: EtOAc/PE (1:1), Rf: 0.2).

1. customThe solvent was evaporated
2. additionthe residue was diluted with water (50 mL)
3. extractionThe product was extracted with EtOAc (2×60 mL)
4. washThe combined organic layer was washed with brine (20 mL)
5. dry with materialdried over anhydrous Na2SO4
6. customevaporated under reduced pressure
7. customThe crude product obtained
8. customwas purified by CC