반응 #61482

반응 방정식

3-acetyl-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine

potassium carbonate

→

title compound

수율 32.0%

7-Methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine

수율 32.0%

용매

hydrochloric acid

반응 조건

후처리

1. 1
   온도at reflux for 18 h
2. 2
   기타the solvent evaporated in vacuo
3. 3
   추출The solid residue was then extracted with ethyl acetate (5×60 ml)
4. 4
   건조the combined organics dried (Na2SO4)
5. 5
   기타The solvent was then evaporated in vacuo

실험 절차

A solution of 3-acetyl-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine (1.75 g, 6.55 mmol) in 5 M hydrochloric acid was heated at reflux for 18 h. The reaction mixture was then cooled to room temperature, basified to pH=12 with potassium carbonate and the solvent evaporated in vacuo. The solid residue was then extracted with ethyl acetate (5×60 ml) and the combined organics dried (Na2SO4). The solvent was then evaporated in vacuo to give the title compound (450 mg, 32%) as a pale yellow oil.

출처