Reaktion #53286

ord-bc3af26e88fd4d6b9caea3c271f731fc

Reaktionsgleichung

CS(=O)(=O)OCc1ccccc1F
2-Fluorobenzyl methanesulfonate
CNCCO
2-(Methylamino)-ethanol
CN(CCO)Cc1ccccc1F
title compound
CN(CCO)Cc1ccccc1F
2-(N-(2-fluorobenzyl)-N-methylamino)-ethanol

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was cooled to room temperature
  2. 2
    Einengenconcentrated
  3. 3
    SonstigeThe crude residue was purified by flash chromatography on silica gel column (chloroform:methanol, 90:10 spiked with triethylamine)

Vorschrift

A mix of 2-Fluorobenzyl methanesulfonate (Step A, 5 g, 24.5 mmol) and 2-(Methylamino)-ethanol (18.4 g, 244.9 mmol) was heated under argon at 120° C. with stirring for 7 hours. The mixture was cooled to room temperature and concentrated. The crude residue was purified by flash chromatography on silica gel column (chloroform:methanol, 90:10 spiked with triethylamine) to provide the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858602B2uspto-grants-2005_02