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Diethylamine → HCID 13385730, Verbindung

HRID 1731955
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1731955
Cl[C:2]1[C:3]2[N:4]([C:12]([C:15]([F:18])([F:17])[F:16])=[N:13][N:14]=2)[C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[CH2:19]([NH:21][CH2:22][CH3:23])[CH3:20]>CN(C)C=O>[CH2:19]([N:21]([CH2:22][CH3:23])[C:2]1[C:3]2[N:4]([C:12]([C:15]([F:18])([F:17])[F:16])=[N:13][N:14]=2)[C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH3:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 8021DiethylamineHCID 14280609HCID 14280609, Verbindung

Produkt 1

HCID 13385730HCID 13385730, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture consisting of 700 mg. (0.0025 mole) of 4-chloro-1-trifluoromethyl-[1,2,4]triazolo[4,3-a]quinoxaline (prepared as described above) and 560 mg. (0.0075 mole) of diethylamine (0.8 ml.) in 10 ml. of N,N-dimethylformamide was stirred at room temperature overnight and then poured over ice. The resulting mixture was then filtered and the recovered solid product washed with water and then dissolved in ethyl acetate. The latter organic solution was next washed with saturated brine and dried over anhydrous magnesium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there are ultimately obtained a light yellow solid which after recrystallization from diethyl ether gave pure 4-diethylamino-1-trifluoromethyl-[1,2,4]triazolo[4,3-a]quinoxaline. The yield of the first crop melting at 155°-157° C. amounted to 260 mg. (34%), while the yield of the second crop melting at 153°-156° C. amounted to 170 mg. (22%).

Aufarbeitung

  1. additionpoured over ice
  2. filtrationThe resulting mixture was then filtered
  3. washthe recovered solid product washed with water
  4. dissolutiondissolved in ethyl acetate
  5. washnext washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customAfter removal of the drying agent
  8. filtrationby means of filtration
  9. customthe solvent by means of evaporation under reduced pressure, there
  10. customare ultimately obtained a light yellow solid which
  11. customafter recrystallization from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-c59ff791f0ab4d6e87d83583c6cbf37d
Quelldatensatz
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04623725

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