Sodium Hydroxide → N-isobutyl-3-bromopyrrolidine-2-one

4.48 g (14.9 mmol) rac-2,4-Dibromo-N-isobutyl-butyramide were dissolved in 40 ml dichloromethane, then 17.3 ml of 50% sodium hydroxide solution and 0.48 g Dowex 2×10 were added. The mixture was stirred vigorously for 4 h at room temperature. Afterwards the mixture was poured into 50 ml ice/water an the phases were separated. The aqueous phase was extracted thrice with 20 ml dichloromethane, and the combined organic phases were washed once with 20 ml water, once with 20 ml brine and dried over magnesium sulfate. After evaporation of the solvent, the resulting colourless oil was chromatographed or silica gel (0.040-0.063 mm) with ethyl acetate/n-hexane 1:1 as eluent.

1. customwere separated
2. extractionThe aqueous phase was extracted thrice with 20 ml dichloromethane
3. washthe combined organic phases were washed once with 20 ml water, once with 20 ml brine
4. dry with materialdried over magnesium sulfate
5. customAfter evaporation of the solvent
6. customthe resulting colourless oil was chromatographed

ORD-Eintrag

ord-f76b08f8a5e247dca48a9237a7c4d875

Quelldatensatz

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05925632