Trifluoroacetic acid → 2-(4-nitro-1H-pyrazol-1-yl)ethanamine-TFA salt

HRID 624026Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 624026
C(OC(=O)[NH:7][CH2:8][CH2:9][N:10]1[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[N:11]1)(C)(C)C.[C:19]([OH:25])([C:21]([F:24])([F:23])[F:22])=[O:20]>C(Cl)Cl>[OH:25][C:19]([C:21]([F:24])([F:23])[F:22])=[O:20].[N+:15]([C:13]1[CH:12]=[N:11][N:10]([CH2:9][CH2:8][NH2:7])[CH:14]=1)([O-:17])=[O:16]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 70984700tert-butyl (2-(4-nitro-1H-pyrazol-1-yl)ethyl)carbamate

Produkt 1

HCID 867042092-(4-nitro-1H-pyrazol-1-yl)ethanamine-TFA salt

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To an ice-cooled solution of tert-butyl(2-(4-nitro-1H-pyrazol-1-yl)ethyl)carbamate (5.50 g, 21.49 mmol) in DCM (55 mL), TFA (20 mL, 261.16 mmol) was added dropwise. The resulting solution was stirred at 0° C. for 3 h, then the reaction mixture was concentrated in vacuo to obtain 2-(4-nitro-1H-pyrazol-1-yl)ethanamine-TFA salt as an off-white paste, which was used in the next step without further purification. LC-MS conditions A: tR=0.21 min, no ionization.

Aufarbeitung

  1. additionwas added dropwise
  2. concentrationthe reaction mixture was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-101cdd90e972465c9332bf01f817215c
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09303023B2

Notizen zur Reaktion

Wird geladen…