反応 #54371

反応方程式

phosphorous tribromide

3-(3-methoxyphenyl)-1-butanol

→

title product

1-bromo-3-(3-methoxyphenyl)butane

溶媒

ether

ether

反応条件

後処理

1. 1
   workup.STIRRINGstirred for an additional 30 minutes
2. 2
   抽出the resulting mixture extracted with ether (3 × 50 ml.)
3. 3
   洗浄The combined extracts are washed with 5% sodium hydroxide solution (3 × 50 ml.), saturated sodium chloride solution (1 × 50 ml.)
4. 4
   乾燥dried (Na2SO4)
5. 5
   その他Removal of the ether and vacuum distillation of the residue

実験手順

A solution of phosphorous tribromide (5.7 ml., 0.06 mole) in ether (30 ml.) is added to a solution of 3-(3-methoxyphenyl)-1-butanol (30.0 g., 0.143 mole) in ether (20 ml.) at -5° C. to -10° C. and the reaction mixture stirred at -5° C. to -10° C. for 2.5 hours. It is then warmed to room temperature and stirred for an additional 30 minutes. The mixture is poured over ice (200 g.) and the resulting mixture extracted with ether (3 × 50 ml.). The combined extracts are washed with 5% sodium hydroxide solution (3 × 50 ml.), saturated sodium chloride solution (1 × 50 ml.) and dried (Na2SO4). Removal of the ether and vacuum distillation of the residue affords the title product.

出典