Triethylamine → N-cyclopropyl-2-nitrobenzenesulfonamide

Temperatur

0 °C

To a solution of cyclopropylamine (1.0 g, 18 mmol) and triethylamine (3.7 mL, 27 mmol) in tetrahydrofuran (20 mL) was added 2-nitrobenzenesulfonyl chloride (3.9 g, 18 mmol) at 0° C., and the mixture was stirred at 0° C. for 1 hour. The solvent was distilled off under reduced pressure, and the residue was diluted with ethyl acetate. The reaction solution was washed with water and saturated brine and dried over magnesium sulfate. The solid was filtered off, and the filtrate was concentrated. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1) and concentrated. The residue was washed with hexane and collected by filtration to obtain the title compound (3.7 g, 87%).

1. distillationThe solvent was distilled off under reduced pressure
2. additionthe residue was diluted with ethyl acetate
3. washThe reaction solution was washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. filtrationThe solid was filtered off
6. concentrationthe filtrate was concentrated
7. customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1)
8. concentrationconcentrated
9. washThe residue was washed with hexane
10. filtrationcollected by filtration

ORD-Eintrag

ord-54aa42dedd6945a3ae83e85f9e326f61

Quelldatensatz

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07795267B2