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Water → HCID 23317237, 화합물

HRID 1982104
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HRID 1982104 반응식
Cl.Cl[CH:3]1[CH2:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:6]=2[N:5]([CH3:22])[CH2:4]1.O.[NH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1>>[Cl:21][C:18]1[CH:19]=[CH:20][C:6]2[N:5]([CH3:22])[CH:3]([CH2:4][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)[CH2:10][N:9]=[C:8]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:7]=2[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 962WaterHCID 8082PiperidineHCID 12318099HCID 12318099, 화합물

생성물 1

HCID 23317237HCID 23317237, 화합물

실험 절차

100 mg of 3,8-dichloro-1-methyl-6-phenyl-1,2,3,4-tetrahydro-1,5-benzodiazocine hydrochloride is heated in 10 ml piperidine under reflux for 24 hours. For processing the mass was poured into water, extracted with chloroform and the chloroform was subsequently distilled off in a vacuum. The product was recrystallized from ether and there was obtained 7-chloro-1-methyl-2-piperidinomethyl-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepine which also was identical with the same material obtained in Examples 4 and 6 of application Ser. No. 355 986 directly by heating acyldiamines with phosphoroxychloride and subsequent reaction with piperidine; m.p. 143°-145° C.

후처리

  1. temperature
under reflux for 24 hours
  • extractionextracted with chloroform
  • distillationthe chloroform was subsequently distilled off in a vacuum
  • customThe product was recrystallized from ether
  • 출처 및 근거

    ORD 기록
    ord-02d0cf505dbb4b4dbd134b3ee12c4f51
    출처 데이터셋
    uspto-grants-1986_06
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04595531

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