Methanesulfonic Acid → 3-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid methanesulfonate

HRID 508055Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 508055
[F:1][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][N:17]3[C:21]([CH2:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:20][C:19]([C:30]4[CH:35]=[CH:34][C:33]([C:36]([F:39])([F:38])[F:37])=[CH:32][CH:31]=4)=[N:18]3)=[CH:12][CH:11]=2)[CH:5]=[CH:4][C:3]=1[CH2:40][CH2:41][C:42]([OH:44])=[O:43].[CH3:45][S:46]([OH:49])(=[O:48])=[O:47]>C(OCC)(=O)C>[CH3:45][S:46]([OH:49])(=[O:48])=[O:47].[F:1][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][N:17]3[C:21]([CH2:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:20][C:19]([C:30]4[CH:31]=[CH:32][C:33]([C:36]([F:38])([F:37])[F:39])=[CH:34][CH:35]=4)=[N:18]3)=[CH:12][CH:11]=2)[CH:5]=[CH:4][C:3]=1[CH2:40][CH2:41][C:42]([OH:44])=[O:43]

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 231574013-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid

Produkt 1

HCID 866243773-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid methanesulfonateAusbeute 60,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 3-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid (500 mg, 0.83 mmol) in ethyl acetate (20 mL) was added methanesulfonic acid (95 mg, 1.0 mmol) at room temperature, and the mixture was stirred for 1 hr. The reaction mixture was concentrated, isopropyl ether was added and the precipitated crystals were collected by filtration, washed with isopropyl ether and dried to give the title compound as colorless crystals (348 mg, yield 60%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. additionisopropyl ether was added
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed with isopropyl ether
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-34d00a36266347b39c113dfdcddfa1ea
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786165B2

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