反応 #6503

ord-eb42087260a94c678501a68bb3d83b03

溶媒

反応条件

温度
10°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A 200 ml flask equipped with a stirrer
  2. 2
    workup.ADDITIONTo the mixture was added dropwise
  3. 3
    その他to precipitate a hydrochloride of triethylamine (white solid)
  4. 4
    workup.ADDITION80 g of hexane was added to complete precipitation of the hydrochloride
  5. 5
    その他The hydrochloride is removed by filteration
  6. 6
    その他condensed

実験手順

A 200 ml flask equipped with a stirrer, a thermometer and a dropping funnel was charged with 14.8 g (0.1 mol) of p-hydroxyethylstyrene, 150 ml of benzene and 10.1 g (0.1 mol) of triethylamine and cooled to 10° C. To the mixture was added dropwise with stirring 13.7 g (0.1 mol) of ethoxalyl chloride for one hour at 10° C. to precipitate a hydrochloride of triethylamine (white solid). After mixting at room temperature for 2 hours, 80 g of hexane was added to complete precipitation of the hydrochloride. The hydrochloride is removed by filteration and the resultant filtrate was condensed to obtain the aimed compound. The compound was identified by 1H NMR (360 Mz) and IR. ##STR7##

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05248749uspto-grants-1993_09