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(R)-1-Phenylpropylamine → HCID 70023804, 화합물

HRID 1358286
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HRID 1358286 반응식
Cl.[Cl:2][C:3]1[C:4]2[NH:15][C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[C:5]=2[N:6]=[CH:7][N:8]=1.C[CH2:17][C@@H:18]([NH2:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>>[ClH:2].[C:19]1([C@H:18]([NH:25][C:3]2[C:4]3[NH:15][C:14]4[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=4[C:5]=3[N:6]=[CH:7][N:8]=2)[CH3:17])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 5324978(R)-1-PhenylpropylamineHCID 181843684-Chloro-5H-pyrimido[5,4-b]indole--hydrogen chloride (1/1)

생성물 1

HCID 70023804HCID 70023804, 화합물수율 11%

실험 절차

4-Chloroindolo[3,2-d]pyrimidine hydrochloride 240 mg, 1 mmol) and (R)-(+)-methylbenzylamine (1 ml) are stirred under a dry nitrogen atmosphere at 150 for 5 hours, and then concentrated under reduced pressure to an oil. This oil is dissolved in EtOAc (20 ml), and stirred for 16 h. The precipitate which forms is collected by filtration, washed with EtOAc, and dried at 90 in vacuo to give 4-([R]-1-phenylethylamino)indolo[3,2-d]pyrimidine hydrochloride (37 mg, 11%). 1H NMR (DMSO): δ10 (1H, s), 9.14 (1H, brs), 8.64 (1H, s), 8.16 (1H, d, J=8.0 Hz), 7.74 (1H, d, J=8.5 Hz), 7.63-7.59 (1H, m), 7.50 (2H, d, J=7.2 Hz), 7.38-7.24 (4H, m), 5.59 (1H, p, J=7.0 Hz); 1.64 (3H, d, J=7.0 Hz).

후처리

  1. concentration
concentrated under reduced pressure to an oil
  • dissolutionThis oil is dissolved in EtOAc (20 ml)
  • filtrationThe precipitate which forms is collected by filtration
  • washwashed with EtOAc
  • customdried at 90 in vacuo
  • 출처 및 근거

    ORD 기록
    ord-e90345f13f0946a8bb8a07ad862bfb6f
    출처 데이터셋
    uspto-grants-2003_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06596726B1

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