반응 #362115

반응 방정식

product

methyl 2-(2-chloro-4-hydroxymethyl-6-propylphenoxy)-2-(3,4-methylenedioxyphenyl)acetate

triphenylphosphine

carbon tetrabromide

→

title compound

methyl 2-(4-bromomethyl-2-chloro-6-propylphenoxy)-2-(3,4-methylenedioxyphenyl)acetate

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타The methylene chloride was then removed in vacuo
3. 3
   세척eluted with 10% EtOAc-hexane
4. 4
   기타Evaporation of the purified fractions
5. 5
   기타drying in vacuo

실험 절차

To a cooled (0°-5° C.), magnetically stirred solution of 0.445 g (1.13 mmol) of the product of step D and 0.446 g (1.70 mmol) of triphenylphosphine dissolved in 5 mL of dichloromethane was added 0.564 g (1.70 mmol) of carbon tetrabromide in several portions. After the addition was complete, the reaction was allowed to warm to room temperature and was stirred an additional 30 minutes. The methylene chloride was then removed in vacuo, and the residue was applied to a silica gel flash chromatography column and eluted with 10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound which was used directly in the next step without further characterization.

출처