反応 #703117

反応方程式

phosphorous oxychloride

trans-(±)-2-amino-4-chloro-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]-quinoline

→

trans-(±)-2-amino-4-chloro-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]quinoline hydrochloride

反応条件

後処理

1. 1
   温度was refluxed with 4 ml
2. 2
   その他formed in the above reaction
3. 3
   workup.ADDITIONwas poured onto ice
4. 4
   ろ過The basic mixture was filtered
5. 5
   workup.DISSOLUTIONthe insoluble material dissolved in 0.1N aqueous hydrochloric acid
6. 6
   その他The hydrochloride salt thus prepared
7. 7
   その他was recrystallized from ethanol

実験手順

The 4-hydroxy product thus obtained was refluxed with 4 ml. of phosphorous oxychloride. The reaction mixture, containing trans-(±)-2-amino-4-chloro-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]-quinoline formed in the above reaction, was poured onto ice and the resulting aqueous mixture made basic. The basic mixture was filtered and the insoluble material dissolved in 0.1N aqueous hydrochloric acid. The hydrochloride salt thus prepared was recrystallized from ethanol to yield trans-(±)-2-amino-4-chloro-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]quinoline hydrochloride having the following physical characteristics. Mass spectrum, molecular ion at 280, smaller peak at 282.

出典