Hydrochloric Acid → HCID 20232116, Verbindung

HRID 2290362Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2290362
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([NH:14][NH2:15])=[N:10][C:9]=2[CH3:16])=[CH:4][CH:3]=1.Cl>C(O)C.[Pd]>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]([CH3:16])[N:10]=[C:11]([NH:14][NH2:15])[NH:12][N:13]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 20232011HCID 20232011, Verbindung

Produkt 1

HCID 20232116HCID 20232116, VerbindungAusbeute 80,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

6-(4-Chlorophenyl)-3-hydrazino-5-methyl-1,2,4-triazine (4.36 g) was dissolved in ethanol (70 ml) containing anhydrous hydrogen chloride, and then hydrogenated over 5% palladium on carbon (0.73 g) under atmospheric pressure at room temperature. After the theoretical amount of hydrogen gas was absorbed, the catalyst was filtered off. The filtrate was evaporated under reduced pressure to give a residual solid, which was recrystallized from diluted hydrochloric acid to give colorless crystals of 6-(4-chlorophenyl)-3-hydrazino-5-methyl-2,5-dihydro-1,2,4-triazine hydrochloride (2.04 g), m.p. 207°~208° C.

Aufarbeitung

  1. customAfter the theoretical amount of hydrogen gas was absorbed
  2. filtrationthe catalyst was filtered off
  3. customThe filtrate was evaporated under reduced pressure
  4. customto give a residual solid, which
  5. customwas recrystallized from diluted hydrochloric acid

Quellen und Nachweise

ORD-Eintrag
ord-23e2b66d3e65456a8bdf8578268ebb46
Quelldatensatz
uspto-grants-1986_10
Patentnummer
US04616014

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