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Triethylamine → 1-(N,N'-Bis(tert-butoxycarbonyl)carbamimidoyl)piperidine-4-carboxylic acid

HRID 1053814
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HRID 1053814 반응식
FC(F)(F)C(O)=O.[NH:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=[O:15])[CH2:10][CH2:9]1.C(N(CC)CC)C.[CH3:24][C:25]([O:28][C:29]([NH:31][C:32](N1C=CC=N1)=[N:33][C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])=[O:30])([CH3:27])[CH3:26]>CO>[CH3:27][C:25]([O:28][C:29]([NH:31][C:32]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=[O:15])[CH2:10][CH2:9]1)=[N:33][C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])=[O:30])([CH3:24])[CH3:26]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 4428040N,N'-Bis(tert-butoxycarbonyl)-1H-pyrazole-1-carboxamidineHCID 90014521Piperidine-4-carboxylic acid trifluoroacetate salt

생성물 1

HCID 1317362991-(N,N'-Bis(tert-butoxycarbonyl)carbamimidoyl)piperidine-4-carboxylic acid수율 76%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of piperidine-4-carboxylic acid trifluoroacetate salt (0.20 g, 0.82 mmol) in methanol (10 mL), triethylamine (0.20 mL, 1.6 mmol) and N,N′-bis{[(2-methyl-2-propanyl)oxy]carbonyl}-1H-pyrazole-1-carboximidamide (0.30 g, 0.98 mmol) was added and the reaction mixture stirred at room temperature for 18 h. The solvent was evaporated under reduced pressure and the resulting residue dissolved in ethyl acetate and washed with brine. The organic layer was dried and concentrated to dryness to obtain the title compound (200 mg, 76%) as a white solid.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe resulting residue dissolved in ethyl acetate
  3. washwashed with brine
  4. customThe organic layer was dried
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-83991b3e84934ade90b87135aac581d9
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394250B2

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