Dimethylformamide diethylacetal → N'-(3-benzylamino-4-cyano-1H-pyrazol-5-yl)-N,N-dimethylformamidine

HRID 1602226Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1602226
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([NH:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:3]=1[C:15]#[N:16].C(O[CH:20](OCC)[N:21]([CH3:23])[CH3:22])C>C1(C)C=CC=CC=1>[CH2:8]([NH:7][C:4]1[C:3]([C:15]#[N:16])=[C:2]([N:1]=[CH:20][N:21]([CH3:23])[CH3:22])[NH:6][N:5]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

Komponenten

4

Edukt 2

HCID 70913Dimethylformamide diethylacetalHCID 108224725-amino-3-benzylamino-1H-pyrazole-4-carbonitrile

Produkt 1

HCID 53832654N'-(3-benzylamino-4-cyano-1H-pyrazol-5-yl)-N,N-dimethylformamidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

Under a N2 atmosphere, a suspension of 74.3 g (348 mmol) of 5-amino-3-benzylamino-1H-pyrazole-4-carbonitrile in 1.0 liter of toluene is boiled under reflux for 2 hours with 70.1 ml (95%; 409 mmol) of N,N-dimethylformamide diethyl acetal. Cooling to RT, filtering with suction and washing with diethyl ether yield N'-(3-benzylamino-4-cyano-1H-pyrazol-5-yl)-N,N-dimethylformamidine; m.p. 197-200° C.; TLC: Rf =0.50 (ethyl acetate).

Aufarbeitung

  1. filtrationfiltering with suction
  2. washwashing with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-3d13961883c1400985aaf7ff4e91bfb3
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05981533

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