反应详情

In a 25 ml flask, under a nitrogen atmosphere, N,N-dimethyl-5-[2-fluoro-5-bromobenzyloxy]pentylamine (696 mg, 1.87 mmol) was dissolved in dichloroethane (6.0 ml). To this solution ACE•Cl (0.305 ml, 2.83 mmol) was added and the resulting mixture was heated to reflux. The reaction mixture was refluxed for twenty hours. The progress of the reaction was monitored by thin layer chromatography. The mixture was refluxed for an additional 16 hours. The solvents were removed in vacuo and the residue was partitioned between 1 M potassium carbonate and methylene chloride. The aqueous fraction was back extracted with methylene chloride. The organic fractions were combined and dried over sodium sulfate. The solvents were removed in vacuo. The title intermediate was further purified by liquid chromatography.

1. temperaturethe resulting mixture was heated to reflux
2. temperatureThe reaction mixture was refluxed for twenty hours
3. temperatureThe mixture was refluxed for an additional 16 hours
4. customThe solvents were removed in vacuo
5. customthe residue was partitioned between 1 M potassium carbonate and methylene chloride
6. extractionThe aqueous fraction was back extracted with methylene chloride
7. dry with materialdried over sodium sulfate
8. customThe solvents were removed in vacuo
9. customThe title intermediate was further purified by liquid chromatography