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Dimethylformamide → HCID 178452358, Verbindung

HRID 1167520
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1167520
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
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

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

Produkt 1

HCID 178452358HCID 178452358, VerbindungAusbeute 78,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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).

Aufarbeitung

  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)

Quellen und Nachweise

ORD-Eintrag
ord-9813c3636085472b841ed701dfd88a14
Quelldatensatz
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06617324B1

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