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Dimethylformamide → HCID 178452358, 화합물

HRID 1167520
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HRID 1167520 반응식
O.[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[NH:13][N:12]=[C:11](C(O)=O)[C:10]=2[C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)=[CH:5][CH:4]=1.ON1C2C=C[CH:31]=[CH:32][C:27]=2N=N1.C([O:37][C:38]([N:40]1[CH2:45]CNC[CH2:41]1)=[O:39])CCC.[CH3:46]N1CCOCC1.[CH3:53][N:54]([CH:56]=[O:57])[CH3:55]>C(OCC)(=O)C>[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[NH:13][N:12]=[C:11]([C:56]([N:54]3[CH2:55][CH2:45][N:40]([C:38]([O:39][C:32]([CH3:31])([CH3:27])[CH3:46])=[O:37])[CH2:41][CH2:53]3)=[O:57])[C:10]=2[C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)=[CH:5][CH:4]=1
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참가 물질

7

반응물 5

HCID 6228DimethylformamideHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 21963126Butyl piperazine-1-carboxylateHCID 178526953HCID 178526953, 화합물

생성물 1

HCID 178452358HCID 178452358, 화합물수율 78.4%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a solution of 5-(4-fluorophenyl)-4-(4-pyridinyl)-1H-pyrazole-3-carboxylic acid, monohydrate prepared in accordance with Example A-200 (0.9905 g, 3.5 mmol) and 1-hydroxybenzotriazole (0.4824 g, 3.57 mmol) in DMF (20 ml) at 0° C. under nitrogen, 1-(3-dimethylaminopropyl)3-ethylcarbodiiminde hydrochloride (0.6984 g, 3.57 mmol, Aldrich Chemical Co.) was added. The solution was stirred at 0° C. under nitrogen for 1 hour then 1-butoxycarbonylpiperazine (0.6585 g, 3.5 mmol) was added followed by N-methylmorpholine (0.40 ml, 3.6 mmol). The reaction was stirred from 0° C. to room temperature overnight. After 19 hours, the solvent was removed under reduced pressure, and resulting residue was diluted with ethyl acetate, washed with saturated NaHCO3 solution, water and brine, and dried over MgSO4. After filtration, the solvent was removed under reduced pressure to give a crude product (1.7595 g). 1,1-Dimethylethyl 4-[[5-(4-fluorophenyl)-4-(4-pyridinyl)-1H-pyrazol-3-yl]carbonyl]-1-piperazinecarboxylate (1.2372 g, 78.4%) was obtained by chromatography. Anal. Calc'd for C24H2N5O3F. (451): C, 63.85; H, 5.80; N, 15.51; Found: C, 63.75; H, 5.71; N, 15.16. MS (MH+): 452 (base peak).

후처리

  1. stirringThe reaction was stirred from 0° C. to room temperature overnight
  2. waitAfter 19 hours
  3. customthe solvent was removed under reduced pressure
  4. customresulting residue
  5. washwashed with saturated NaHCO3 solution, water and brine
  6. dry with materialdried over MgSO4
  7. filtrationAfter filtration
  8. customthe solvent was removed under reduced pressure
  9. customto give a crude product (1.7595 g)

출처 및 근거

ORD 기록
ord-9813c3636085472b841ed701dfd88a14
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06617324B1

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