Trifluoroacetic acid → 4-[4-Carbamoyl-3-(phenylamino)-1H-pyrazol-1-yl]-4-(cyanomethyl)piperidinium trifluoroacetate

HRID 521222Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 521222
[C:1]([C:4]1[C:5]([NH:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[N:6][N:7]([C:9]2([CH2:22][C:23]#[N:24])[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]2)[CH:8]=1)(=[O:3])[NH2:2].[C:32]([OH:38])([C:34]([F:37])([F:36])[F:35])=[O:33]>C(Cl)Cl>[F:35][C:34]([F:37])([F:36])[C:32]([O-:38])=[O:33].[C:1]([C:4]1[C:5]([NH:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[N:6][N:7]([C:9]2([CH2:22][C:23]#[N:24])[CH2:14][CH2:13][NH2+:12][CH2:11][CH2:10]2)[CH:8]=1)(=[O:3])[NH2:2]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 71536247tert-Butyl 4-[4-carbamoyl-3-(phenylamino)-1H-pyrazol-1-yl]-4-(cyanomethyl)piperidine-1-carboxylate

Produkt 1

HCID 867293834-[4-Carbamoyl-3-(phenylamino)-1H-pyrazol-1-yl]-4-(cyanomethyl)piperidinium trifluoroacetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a suspension of tert-butyl 4-[4-carbamoyl-3-(phenylamino)-1H-pyrazol-1-yl]-4-(cyanomethyl)piperidine-1-carboxylate (2.0 g, 4.7 mmol) in DCM (20 mL) was added TFA (5.0 mL) dropwise. The resultant clear solution was maintained at ambient temperature for 1.5 hours. The mixture was then concentrated in vacuo, and the residue was dissolved in a mixture of MeCN/water (35 mL:15 mL) and lyophilized to afford the title compound, Example #38-1.

Aufarbeitung

  1. concentrationThe mixture was then concentrated in vacuo
  2. dissolutionthe residue was dissolved in a mixture of MeCN/water (35 mL:15 mL)

Quellen und Nachweise

ORD-Eintrag
ord-62e21296db404c3cb0a66c10d5e0e97c
Quelldatensatz
uspto-grants-2016_05
Patentnummer
US09328099B2

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