反应详情

2,5-Dihydro-pyrrole-1-carboxylic acid tert-butyl ester (46 g, 65% purity) was dissolved in CH2Cl2 (500 mL). The solution was cooled to 0° C. mCPBA (122 g, 2 eq, 77% purity) was slowly added to the solution at 0° C. The reaction mixture was stirred at 0° C. to RT for overnight. The mixture was concentrated to 200 ml, and filtered. The organic phase was washed with 1 N NaOH solution (4×100 mL), dried over Na2SO4. The resulting oil was purified by column chromatography (hexane:ethyl acetate 3:1) to give 28 g of desired product as a colorless oil (87% yield). 1H-NMR (300 MHz, CDCl3): δ 1.41 (s, 9H), 3.26 (dd, 2H), 3.25-3.80 (m, 4H)

1. additionwas slowly added to the solution at 0° C
2. concentrationThe mixture was concentrated to 200 ml
3. filtrationfiltered
4. washThe organic phase was washed with 1 N NaOH solution (4×100 mL)
5. dry with materialdried over Na2SO4
6. customThe resulting oil was purified by column chromatography (hexane:ethyl acetate 3:1)