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Trifluoroacetic acid → HCID 22029751, 화합물

HRID 1792078
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HRID 1792078 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH:9]1[CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[N:28]1[C:36]2[C:35](=[O:37])[N:34]([CH3:38])[C:33](=[O:39])[N:32]([CH3:40])[C:31]=2[N:30]=[CH:29]1)=O)(C)(C)C.[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44]>>[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44].[CH3:40][N:32]1[C:31]2[N:30]=[C:29]3[N:28]([C:36]=2[C:35](=[O:37])[N:34]([CH3:38])[C:33]1=[O:39])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[CH2:21][CH:9]1[CH2:10][NH:11][CH2:12][CH2:13][N:8]31
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 23536894HCID 23536894, 화합물

생성물 1

HCID 22029751HCID 22029751, 화합물

실험 절차

2-[2-(1,3-dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-7-yl)benzyl]piperazine-1,4-dicarboxylic acid di-tert-butyl ester (0.055 g) was dissolved in trifluoroacetic acid (0.5 ml), the mixture was stirred for 30 minutes, and the solvent was removed by distillation at reduced pressure. The residue was dissolved in N,N-dimethylformamide, and N-chlorosuccinimide (0.025 g) was added to the solution. The mixture was stirred at room temperature for 14 hours, 1,8-diazabicyclo-[5,4,0]-7-undecene (0.050 ml) was added thereto, and was further stirred for 1 hour. After removing the solvent by distillation at reduced pressure, the residue was purified by HPLC with a reversed phase column using water-acetonitrile-trifluoroacetic acid system as elution solvent to give 0.0079 g of the title compound.

후처리

  1. customthe solvent was removed by distillation at reduced pressure
  • dissolutionThe residue was dissolved in N,N-dimethylformamide
  • additionN-chlorosuccinimide (0.025 g) was added to the solution
  • stirringThe mixture was stirred at room temperature for 14 hours
  • addition1,8-diazabicyclo-[5,4,0]-7-undecene (0.050 ml) was added
  • stirringwas further stirred for 1 hour
  • customAfter removing the solvent
  • distillationby distillation at reduced pressure
  • customthe residue was purified by HPLC with a reversed phase column
  • washas elution solvent
  • 출처 및 근거

    ORD 기록
    ord-ab99aab08c6b4fb0ae2b6f9fa5a52a16
    출처 데이터셋
    uspto-grants-2006_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07074798B2

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