반응 #367772

반응 방정식

3-methylbenzo[b]thiophene-6-carboxylic acid methyl ester

N-bromosuccinimide

azobisisobutyronitrile

→

3-bromomethylbenzo[b]thiophene-6-carboxylic acid methyl ester

수율 56.2%

용매

carbon tetrachloride

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 2 hours
3. 3
   온도cooled
4. 4
   workup.ADDITIONThe mixture was diluted with a few ml
5. 5
   세척of chloroform, washed with water
6. 6
   건조dried (Na2SO4)
7. 7
   기타evaporated
8. 8
   기타to give a solid which
9. 9
   기타was crystallized from ethyl acetate/petrol (b.p. 60°-80° C.)

실험 절차

A mixture of 3-methylbenzo[b]thiophene-6-carboxylic acid methyl ester (1.03 g), N-bromosuccinimide (0.89 g), azobisisobutyronitrile (0.2 g) and carbon tetrachloride (25 ml) was heated under reflux for 2 hours and then cooled. The mixture was diluted with a few ml. of chloroform, washed with water, dried (Na2SO4) and evaporated to give a solid which was crystallized from ethyl acetate/petrol (b.p. 60°-80° C.) to give 3-bromomethylbenzo[b]thiophene-6-carboxylic acid methyl ester (0.80 g), m.p. 108°-110° C.

출처