Water → (5-chloro-1,3-dimethyl-1H-pyrazol-4-yl)methanamine hydrochloride

HRID 530794Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 530794
[N:1]([CH2:4][C:5]1[C:6]([CH3:12])=[N:7][N:8]([CH3:11])[C:9]=1[Cl:10])=[N+]=[N-].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O.[NH4+].[OH-]>C1COCC1>[ClH:10].[Cl:10][C:9]1[N:8]([CH3:11])[N:7]=[C:6]([CH3:12])[C:5]=1[CH2:4][NH2:1]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11776TriphenylphosphineHCID 14923Ammonium HydroxideHCID 613734544-(azidomethyl)-5-chloro-1,3-dimethyl-1H-pyrazole

Produkt 1

HCID 90419183(5-chloro-1,3-dimethyl-1H-pyrazol-4-yl)methanamine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of compound 3 (175 mg, 0.95 mmol) in THF (5 mL) was added PPh3 (248 mg, 0.95 mmol) at 0° C. After stirring for 1 hr, water (0.03 mL) and NH4OH (0.07 mL) were added sequentially and the resulting mixture was stirred at room temperature for overnight. After the solvent was evaporated, the residue was purified with reversed flash to give a white solid. LCMS (ESI) m/z=160 (M+H)+.

Aufarbeitung

  1. stirringthe resulting mixture was stirred at room temperature for overnight
  2. customAfter the solvent was evaporated
  3. customthe residue was purified with reversed flash
  4. customto give a white solid

Quellen und Nachweise

ORD-Eintrag
ord-db7c4232359642ff99323cbe14e94601
Quelldatensatz
uspto-grants-2016_05
Patentnummer
US09353104B2

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