反应详情

6 gm (31.3 mmols) of 2-amino-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine were dissolved in 100 ml of glacial acetic acid and, while cooling the solution with ice, chlorine was introduced until the thin-layer chromatogram showed that no more starting material was present. Thereafter, the reaction mixture was made alkaline with 2N sodium hydroxide and was then extracted with chloroform. The chloroform extract solution was evaporated, and the residue was column-chromatographically purified on silicagel with ethyl acetate/methanol/ethanolic ammonia (4:1:0.5) as the mobile phase. The hydrochloride was precipitated from ethanol with ethanolic hydrochloric acid.

1. additionwas introduced until the thin-layer chromatogram
2. extractionwas then extracted with chloroform
3. extractionThe chloroform extract solution
4. customwas evaporated
5. custompurified on silicagel with ethyl acetate/methanol/ethanolic ammonia (4:1:0.5) as the mobile phase
6. customThe hydrochloride was precipitated from ethanol with ethanolic hydrochloric acid