반응 #1807520

반응 방정식

bromine

2-[2'-(1H-tetrazol-5-yl)-phenyl]-5-methylbenzofuran

cyclohexene

→

3-bromo-2-[2'-(1H-tetrazol-5-yl)-phenyl]-5-methylbenzofuran

용매

carbon tetrachloride

dioxane

반응 조건

후처리

1. 1
   농축the reaction mixture is concentrated by evaporation in vacuo
2. 2
   추출extracted with 100 ml of ether
3. 3
   기타The two lower phases are separated off
4. 4
   추출extracted three times with 100 ml of ethyl acetate each time
5. 5
   세척The combined ethyl acetate phases are washed with 100 ml of brine
6. 6
   기타after removal of the solvent in vacuo, they
7. 7
   기타result in a yellow oil which

실험 절차

A solution of 11.6 g of bromine in 28 ml of carbon tetrachloride is added dropwise over the course of 35 minutes to a suspension of 10.0 g of 2-[2'-(1H-tetrazol-5-yl)-phenyl]-5-methylbenzofuran in 418 ml of dioxane. After stirring for 3 hours at room temperature, 12.6 ml of cyclohexene are added dropwise and then the reaction mixture is concentrated by evaporation in vacuo. The residue is taken up in 50 ml of 2N sodium hydroxide solution and extracted with 100 ml of ether. Three clear phases form. The two lower phases are separated off, acidified with 40 ml of 4N hydrochloric acid and extracted three times with 100 ml of ethyl acetate each time. The combined ethyl acetate phases are washed with 100 ml of brine and, after removal of the solvent in vacuo, they result in a yellow oil which yields crystalline 3-bromo-2-[2'-(1H-tetrazol-5-yl)-phenyl]-5-methylbenzofuran, m.p. 167°-168°, from toluene.

출처