反应详情

37% Hydrochloric acid (1 mL) was added to a stirred solution of 2-methyl-2-nitro-1-phenylpropan-1-ol (26c, 0.12 g, 0.6 mmol in EtOH (10 mL) and water (5 mL). Zinc powder (0.241 g, 3.6 mmol) was slowly added in small portions, the mixture was stirred for 4 hours at +70° C. The mixture was filtered to remove solid zinc residues and concentrated to ⅓ volume by evaporation, diluted with water (50 mL) and washed with ether (125 mL). The acidic waterphase was made basic using KOH (aq) solution, the formed slurry was extracted with ether (3×150 mL). The organic phase was dried (MgSO4) filtered and evaporated. The crude product was further purified by HPLC. Yield 60 mg (60%).

1. filtrationThe mixture was filtered
2. customto remove solid zinc residues
3. concentrationconcentrated
4. customby evaporation
5. additiondiluted with water (50 mL)
6. washwashed with ether (125 mL)
7. extractionthe formed slurry was extracted with ether (3×150 mL)
8. dry with materialThe organic phase was dried (MgSO4)
9. filtrationfiltered
10. customevaporated
11. customThe crude product was further purified by HPLC