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1-Phenylpiperazine → HCID 57682692, 화합물

HRID 494253
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HRID 494253 반응식
[C:1](OC(OC(OC(C)(C)C)=O)=O)(OC(C)(C)C)=[O:2].[NH2:19][C:20]1[CH:29]=[C:28]2[C:23]([CH:24]=[CH:25][CH:26]=[N:27]2)=[CH:22][CH:21]=1.C(F)(F)(C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)N(C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F.[C:79]1([N:85]2[CH2:90][CH2:89][NH:88][CH2:87][CH2:86]2)[CH:84]=[CH:83][CH:82]=[CH:81][CH:80]=1>C(Cl)Cl>[C:79]1([N:85]2[CH2:90][CH2:89][N:88]([C:1]([NH:19][C:20]3[CH:29]=[C:28]4[C:23]([CH:24]=[CH:25][CH:26]=[N:27]4)=[CH:22][CH:21]=3)=[O:2])[CH2:87][CH2:86]2)[CH:84]=[CH:83][CH:82]=[CH:81][CH:80]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 70961-PhenylpiperazineHCID 113777-AminoquinolineHCID 67646PerfluorotripentylamineHCID 11780301Di-tert-butyl tricarbonate

생성물 1

HCID 57682692HCID 57682692, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of di-tert-butyl tricarbonate (60 mg, 0.23 mmol) in DCM (1 ml) was added in one portion, a solution of 7-aminoquinoline (D55) (30 mg, 0.21 mmol) in DCM (1 ml). After 5 mins, when gas evolution was complete, tris -amine resin (12 mg 0.04 mmol) was added, then after 1 h a solution of 4-phenylpiperazine (32 ul, 0.21 mmol) was added and the reaction stirred at room temperature overnight. The reaction mixture was then purified directly by SPE column chromatography, eluting with an EtOAc/60-80° C.-petroleum ether gradient, followed by treatment with excess methyl isocyanate resin to remove unreacted 7-aminoquinoline starting material from the product. On completion the resin was removed by filtration and filtrate concentrated in vacuo to give the title compound as an orange gum. 1H NMR (250 MHz, CDCl3) δ (ppm): 8.85 (dd, 1H), 8.09 (dd, 1H), 7.93 (dd, 1H), 7.82 (s, 1H), 7.76 (d, 1H), 7.30 (m, 3H), 6.94 (m, 3H), 6.83 (br, 1H), 3.72 (m, 4H), 3.28 (m, 4H).

후처리

  1. customThe reaction mixture was then purified directly by SPE column chromatography
  2. washeluting with an EtOAc/60-80° C.-petroleum ether gradient
  3. customto remove unreacted 7-aminoquinoline starting material from the product
  4. customOn completion the resin was removed by filtration and filtrate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3e53c10e6c4b40d3ba3a9925b371c1af
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538121B2

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