反应详情

To a suspension of 1-benzhydryl-4-(3-((phenylsulfonyl)methyl)oxetan-3-yl)piperazine (2.49 g, 5.38 mmol) in MeOH (50 mL), THF (10 mL) was added MAGNESIUM (0.654 g, 26.9 mmol) which was pretreated with 1.0 N HCl and rinsed with MeOH, stirred at rt overnight. The Et2O was added and followed by Na2SO4.10H2O, stirred at room temperature for 1 hr, filtered, and filtrate was concentrated. The crude was purified by 40 g ISCO silica column, eluted with EA: HX-0-100%, the desired fractions were concentrated to yield 1-benzhydryl-4-(3-methyloxetan-3-yl)piperazine (1.08 g) as a white solid.

1. washrinsed with MeOH
2. additionThe Et2O was added
3. stirringstirred at room temperature for 1 hr
4. filtrationfiltered
5. concentrationfiltrate was concentrated
6. customThe crude was purified by 40 g ISCO silica column
7. washeluted with EA
8. concentrationHX-0-100%, the desired fractions were concentrated