Phosphorus oxychloride → HCID 18596278, 화합물

HRID 745521노트

반응식

HRID 745521 반응식
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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 18596258HCID 18596258, 화합물

생성물 1

HCID 18596278HCID 18596278, 화합물

실험 절차

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.

후처리

  1. temperaturewas refluxed with 4 ml
  2. customformed in the above reaction
  3. additionwas poured onto ice
  4. filtrationThe basic mixture was filtered
  5. dissolutionthe insoluble material dissolved in 0.1N aqueous hydrochloric acid
  6. customThe hydrochloride salt thus prepared
  7. customwas recrystallized from ethanol

출처 및 근거

ORD 기록
ord-e8ea720f14bc416ab5011486651be7d6
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599339

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