반응 #1766546

반응 방정식

5-methyl-1,2,4,5-tetrahydro-3H-2-benzazepin-3-one

acrylonitrile

hydrochloric acid

benzyltrimethylammonium hydroxide

→

2-(2-cyanoethyl)-5-methyl-1,2,4,5-tetrahydro-3H-2-benzazepin-3-one

용매

water

pyridine

pyridine

반응 조건

후처리

1. 1
   workup.ADDITIONTo a mixture of 6 g
2. 2
   추출extracted with chloroform
3. 3
   세척The organic phase is washed neutral with water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   여과It is filtered
6. 6
   기타the solvent is evaporated off in vacuo

실험 절차

To a mixture of 6 g. (0.034 moles) of 5-methyl-1,2,4,5-tetrahydro-3H-2-benzazepin-3-one and 4 drops of Triton B (benzyltrimethylammonium hydroxide) in 10 ml. of pyridine, are added dropwise 2 g. (0.038 moles) of acrylonitrile dissolved in 2.5 ml. of pyridine. The reaction mixture is heated to 80° C. for 2 hours and then poured into iced water. It is acidified with hydrochloric acid to pH 4 and extracted with chloroform. The organic phase is washed neutral with water and then dried over anhydrous sodium sulfate. It is filtered and the solvent is evaporated off in vacuo. 8 g. (almost theoretical yield) of syrupy 2-(2-cyanoethyl)-5-methyl-1,2,4,5-tetrahydro-3H-2-benzazepin-3-one are obtained.

출처