Reaktion #684952

ord-7663ec31b19a44d0b3295f79ec346672

Reaktionsgleichung

O=C([O-])O.[Na+]
sodium hydrogencarbonate
CS(=O)(=O)Cl
Methanesulfonyl chloride
CCN(CC)CC
triethylamine
OCc1ccccc1I
o-iodobenzyl alcohol
ClCc1ccccc1I
title compound
Ausbeute 100.7%
ClCc1ccccc1I
1-(Chloromethyl)-2-iodobenzene
Ausbeute 100.7%

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe resulting mixture was extracted with methylene chloride
  2. 2
    TrocknenThe methylene chloride layer was dried over anhydrous magnesium sulfate
  3. 3
    Einengenconcentrated under reduced pressure

Vorschrift

Methanesulfonyl chloride (2.0 ml, 29 mmol) and triethylamine (3.6 ml, 26 mmol) were added to a solution of o-iodobenzyl alcohol (5.0 g, 21 mmol) in methylene chloride (50 ml) cooled to 0° C., and the mixture was stirred at that temperature for 19 hours. A 5% aqueous sodium hydrogencarbonate solution was added, and the resulting mixture was extracted with methylene chloride. The methylene chloride layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give the title compound (5.34 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07897387B2uspto-grants-2011_03