반응 #47813

반응 방정식

6-Methyl-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester

6-methyl-1-oxo-3-phenyl-1H-indene-2-carboxylic Acid Ethyl Ester

N-bromosuccinimide

2,2′-azobisisobutyronitrile

→

titled compound

수율 36.7%

6-bromomethyl-1-oxo-3-phenyl-1H-indene-2-carboxylic Acid Ethyl Ester

수율 36.7%

용매

carbon tetrachloride

반응 조건

후처리

1. 1
   기타Upon the completion of the reaction
2. 2
   세척the resulting mixture washed with saturated saline
3. 3
   추출extracted with dichloromethane
4. 4
   기타The organic layer was separated
5. 5
   건조dried over anhydrous MgSO4
6. 6
   농축concentrated under a reduced pressure
7. 7
   기타The resulting residue was purified by flash chromatography

실험 절차

6-Methyl-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (3 g, 10.3 mmol) obtained in Step 4 was dissolved in carbon tetrachloride, and N-bromosuccinimide (2 g, 11.4 mmol) and 2,2′-azobisisobutyronitrile (500 mg, 3.09 mmol) were added thereto. The mixture was refluxed for 3 hrs under the irradiation of a 375 W tungsten lamp. Upon the completion of the reaction, the resulting mixture washed with saturated saline and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 1.4 g of the titled compound (yield: 36.7%) in oil state.

출처