Dimethylformamide diethylacetal → N'-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine

HRID 1068890

Reaktionsgleichung

Reaktionsgleichung von HRID 1068890
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([N:7]2[CH2:12][CH2:11][O:10][CH2:9][CH2:8]2)[C:3]=1[C:13]#[N:14].C(O[CH:18](OCC)[N:19]([CH3:21])[CH3:20])C>C1(C)C=CC=CC=1>[N:7]1([C:4]2[C:3]([C:13]#[N:14])=[C:2]([N:1]=[CH:18][N:19]([CH3:21])[CH3:20])[NH:6][N:5]=2)[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1

Komponenten

4

Edukt 2

HCID 70913Dimethylformamide diethylacetalHCID 49626575-amino-3-(morpholin-4-yl)-1H-pyrazole-4-carbonitrile

Produkt 1

HCID 54020168N'-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

Under a nitrogen atmosphere, a suspension of 4.00 g (20.7 mmol) of 5-amino-3-(morpholin-4-yl)-1H-pyrazole-4-carbonitrile in 85 ml of toluene is boiled under reflux for 5 hours with 4.17 ml (97%; 23.6 mmol) of N,N-dimethylformamide diethyl acetal, during which the solid dissolves. Cooling to RT (→crystallization), filtration with suction an d washing with toluene and hexane yield N′-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine; m.p. 182-183° C.; TLC: Rf=0.20 (ethyl acetate).

Aufarbeitung

  1. dissolutiondissolves
  2. filtration(→crystallization), filtration with suction
  3. washan d washing with toluene and hexane

Quellen und Nachweise

ORD-Eintrag
ord-2267d8654dfb42d1ab8ac664cd0cce9e
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06251911B1

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