反应详情

To a solution of tert-butyl α-hydroxyisobutyrate (533 mg, 3.32 mmol) in 4.5 mL DMF and 0.75 mL THF was added portion wise (133 mg, 3.32 mmol) sodium hydride at room temperature. After the reaction mixture had been stirring for 15 minutes, a solution of 2-(5-bromo-2-fluoro-phenyl)-2-difluoromethyl-1-(2-nitro-benzenesulfonyl)-aziridine (1 g, 2.22 mmol) was added. The reaction mixture was stirred at rt for 150 minutes and quenched with aqueous NH4Cl solution. TBME was added, the layers were separated, washed with brine and TBME. The combined organic layers were dried over MgSO4.H2O and evaporated. The crude product was purified on a silica gel column by eluting with hexane/EtOAc 6/1->5/1 to give 1.10 g of the title compound as a pale yellow resin.

1. stirringThe reaction mixture was stirred at rt for 150 minutes
2. customquenched with aqueous NH4Cl solution
3. additionTBME was added
4. customthe layers were separated
5. washwashed with brine and TBME
6. dry with materialThe combined organic layers were dried over MgSO4.H2O
7. customevaporated
8. customThe crude product was purified on a silica gel column
9. washby eluting with hexane/EtOAc 6/