反应详情

To a suspension of 2-methyl-2-nitro-1-propanol (2.3975 g, 20.13 mmol) and Ag2O (4.6385 g, 20.02 mmol) in DMF (25 ml) was added benzyl bromide (2.65ml, 22.28 mmol) and stirred for 48 hours. The mixture was filtered and the filtrate was added to 5% KHSO4 aqueous solution, extracted three times with ethyl acetate/hexane=1/1 and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (toluene) to give the title compound (639.4 mg; 15%).

1. filtrationThe mixture was filtered
2. additionthe filtrate was added to 5% KHSO4 aqueous solution
3. extractionextracted three times with ethyl acetate/hexane=1/1
4. dry with materialdried over MgSO4
5. concentrationThe mixture was concentrated
6. custompurified by silica gel chromatography (toluene)