Potassium Carbonate → HCID 17973671, 화합물

HRID 1366982노트

반응식

HRID 1366982 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][C:15](O)=O)=O)(C)(C)C.[F:18][C:19]1[CH:20]=[C:21]([NH2:27])[C:22]([NH2:26])=[CH:23][C:24]=1[F:25].C(=O)([O-])[O-].[K+].[K+]>>[F:18][C:19]1[C:24]([F:25])=[CH:23][C:22]2[NH:26][C:15]([CH2:14][CH:9]3[CH2:10][CH2:11][CH2:12][CH2:13][NH:8]3)=[N:27][C:21]=2[CH:20]=1

참가 물질

4

반응물 3

HCID 11430Potassium CarbonateHCID 27367551,2-Diamino-4,5-difluorobenzeneHCID 50585361-Boc-2-Piperidineacetic Acid

생성물 1

HCID 17973671HCID 17973671, 화합물수율 69.3%

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온도
140 °C

실험 절차

A mixture of 2-carboxymethyl-piperidine-1-carboxylic acid tert-butyl ester (Beckett et al, J. Med. Chem., 563, 1969) (10.0 g, 41 mmol) and 4,5-difluoro-benzene-1,2-diamine (5.95 g, 41 mmol) in polyphosphoric acid (140 g) was heated at 140° C. for 7 h. The cooled reaction mixture was poured onto excess solid potassium carbonate and crushed ice. The resulting basic, aqueous solution was extracted with ethyl acetate (2×) and the combined organics were washed with brine, dried (Na2SO4) and the solvent removed in vacuo. The residue was triturated with diethyl ether, ethyl acetate and pentane to afford the title compound as a light brown solid (7.14 g, 69%).

후처리

  1. customThe cooled reaction mixture
  2. customcrushed ice
  3. extractionThe resulting basic, aqueous solution was extracted with ethyl acetate (2×)
  4. washthe combined organics were washed with brine
  5. dry with materialdried (Na2SO4)
  6. customthe solvent removed in vacuo
  7. customThe residue was triturated with diethyl ether, ethyl acetate and pentane

출처 및 근거

ORD 기록
ord-73e11bce3f0147cc9bd53568de00ffc7
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07893090B2

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