反応 #2069945

ord-508a273364064d978063b74569dc395b

反応方程式

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

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the resulting mixture was extracted with methylene chloride
  2. 2
    乾燥The methylene chloride layer was dried over anhydrous magnesium sulfate
  3. 3
    濃縮concentrated under reduced pressure

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07541332B2uspto-grants-2009_06