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Hydrochloride methanol → HCID 67958029, 화합물

HRID 1529356
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HRID 1529356 반응식
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]2[N:20]=[C:19]([C:21]3[C:29]4[C:24](=[CH:25][CH:26]=[C:27]([N+:30]([O-:32])=[O:31])[CH:28]=4)[N:23](C(OC(C)(C)C)=O)[CH:22]=3)[CH:18]=[N:17][CH:16]=2)[CH2:11][CH2:10]1)=O)(C)(C)C.CO.Cl>>[N+:30]([C:27]1[CH:28]=[C:29]2[C:24](=[CH:25][CH:26]=1)[NH:23][CH:22]=[C:21]2[C:19]1[N:20]=[C:15]([N:12]2[CH2:11][CH2:10][CH:9]([NH2:8])[CH2:14][CH2:13]2)[CH:16]=[N:17][CH:18]=1)([O-:32])=[O:31]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 21893726Hydrochloride methanolHCID 67959775HCID 67959775, 화합물

생성물 1

HCID 67958029HCID 67958029, 화합물수율 23.1%

반응 조건

온도
60 °C

실험 절차

To tert-butyl 3-(6-(4-(tert-butoxycarbonylamino)piperidin-1-yl)pyrazin-2-yl)-5-nitro-1H-indole-1-carboxylate (170 mg, 0.32 mmol) was added 3N MeOH—HCl (3.5 mL) and then heated at 60° C. overnight. The reaction mixture was quenched with water and neutralized with K2CO3. The resulting precipitate was filtered, washed with water and dried to obtain the crude compound. This crude compound was re-crystallized in ethanol to obtain the title compound as a pale yellow solid (25 mg). MS (ESI, pos. ion) m/z: 339.1 (M+1).

후처리

custom
The reaction mixture was quenched with water and neutralized with K2CO3
  • filtrationThe resulting precipitate was filtered
  • washwashed with water
  • customdried
  • customto obtain the crude compound
  • customThis crude compound was re-crystallized in ethanol
  • 출처 및 근거

    ORD 기록
    ord-3cd7b9fad8c642d2887f668837b26042
    출처 데이터셋
    uspto-grants-2015_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09090593B2

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