Triphenylphosphine → 2-methyl-2-(4-nitro-1H-pyrazol-1-yl)propan-1-amine

HRID 714834Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 714834
[N:1]([CH2:4][C:5]([N:8]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[N:9]1)([CH3:7])[CH3:6])=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1.O>[CH3:7][C:5]([N:8]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[N:9]1)([CH3:6])[CH2:4][NH2:1]

Komponenten

4

Edukt 2

HCID 11776TriphenylphosphineHCID 1178402371-(1-azido-2-methylpropan-2-yl)-4-nitro-1H-pyrazole

Produkt 1

HCID 825041082-methyl-2-(4-nitro-1H-pyrazol-1-yl)propan-1-amineAusbeute 99,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21881883Oxolane--water (1/1)Lösungsmittel

Versuchsvorschrift

To a solution of 1-(1-azido-2-methylpropan-2-yl)-4-nitro-1H-pyrazole (10 g) obtained in Step C of Example 115 in a mixed solvent of tetrahydrofuran/water (v/v=10/1, 88 mL) was added triphenylphosphine (15 g), and the mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give the title compound (8.7 g) as a mixture with triphenylphosphine oxide.

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (ethyl acetate/methanol)

Quellen und Nachweise

ORD-Eintrag
ord-f42104d714724122bd1f495aca85cfbd
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09187453B2

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