反应 #684952

ord-7663ec31b19a44d0b3295f79ec346672

反应方程式

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

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the resulting mixture was extracted with methylene chloride
  2. 2
    干燥The methylene chloride layer was dried over anhydrous magnesium sulfate
  3. 3
    浓缩concentrated under reduced pressure

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07897387B2uspto-grants-2011_03