반응 #54371

반응 방정식

phosphorous tribromide

3-(3-methoxyphenyl)-1-butanol

→

title product

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

용매

ether

ether

반응 조건

후처리

1. 1
   workup.STIRRINGstirred for an additional 30 minutes
2. 2
   추출the resulting mixture extracted with ether (3 × 50 ml.)
3. 3
   세척The combined extracts are washed with 5% sodium hydroxide solution (3 × 50 ml.), saturated sodium chloride solution (1 × 50 ml.)
4. 4
   건조dried (Na2SO4)
5. 5
   기타Removal of the ether and vacuum distillation of the residue

실험 절차

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.

출처