Triethylamine → 3-{4-[(Tert-butoxycarbonyl)amino]phenyl}propyl methanesulfonate

A mixture of 3-(4-tert-butoxycarbonylaminophenyl)propanol (2.66 g, 10.6 mmol), methanesulfonylchloride (1.33 g, 11.6 mmol), triethylamine (1.18 g, 11.7 mmol) and ethyl acetate (10 ml) was stirred at room temperature for 1 hour. Then the reaction mixture was diluted with ethyl acetate and successively washed with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was chromatographed on silica gel (50 g) with hexane-ethyl acetate (3:1) to give 3-(4-tert-butoxycarbonylaminophenyl)propyl methanesulfonate as colorless crystals (2.75 g, 79%).

1. washsuccessively washed with water and brine
2. dry with materialdried over MgSO4
3. concentrationconcentrated in vacuo
4. customThe residue was chromatographed on silica gel (50 g) with hexane-ethyl acetate (3:1)

ORD-Eintrag

ord-723105fe2fa64ad4a6cdbefe76dd0afd

Quelldatensatz

uspto-grants-2001_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06235731B1