Phosphorus oxychloride → HCID 18596278、化合物
反応式
P(Cl)(Cl)([Cl:3])=O.[NH2:6][C:7]1[N:8]=[C:9]([Cl:24])[C:10]2[CH2:19][C@H:18]3[C@@H:13]([CH2:14][CH2:15][CH2:16][N:17]3[CH2:20][CH2:21][CH3:22])[CH2:12][C:11]=2[N:23]=1>>[ClH:3].[NH2:6][C:7]1[N:8]=[C:9]([Cl:24])[C:10]2[CH2:19][C@H:18]3[C@@H:13]([CH2:14][CH2:15][CH2:16][N:17]3[CH2:20][CH2:21][CH3:22])[CH2:12][C:11]=2[N:23]=1参加物
3
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.
後処理
- temperaturewas refluxed with 4 ml
- customformed in the above reaction
- additionwas poured onto ice
- filtrationThe basic mixture was filtered
- dissolutionthe insoluble material dissolved in 0.1N aqueous hydrochloric acid
- customThe hydrochloride salt thus prepared
- customwas recrystallized from ethanol
出典と根拠
- ORDレコード
- ord-e8ea720f14bc416ab5011486651be7d6
- 出典データセット
- uspto-grants-1986_07
- 特許番号
- US04599339
反応ノート
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