HCID 20232011, Verbindung → HCID 15586410, Verbindung

HRID 2290363Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2290363
[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.ICS[C:20]1[NH:21][CH2:22][CH2:23][N:24]=1>C(O)CCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:13]=[N:12][C:11]([NH:14][NH:15][C:20]3[NH:24][CH2:23][CH2:22][N:21]=3)=[N:10][C:9]=2[CH3:16])=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 20232011HCID 20232011, VerbindungHCID 20232073HCID 20232073, Verbindung

Produkt 1

HCID 15586410HCID 15586410, VerbindungAusbeute 17 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

A mixture of 6-(4-chlorophenyl)-3-hydrazino-5-methyl-1,2,4-triazine (7 g), 2-iodomethylthio-2-imidazoline (8.11 g) and n-butanol (50 ml) was refluxed for 3 hours with stirring. After cooling, the mixture was evaporated under reduced pressure and the residue was dissolved in 1N hydrochloric acid. The solution was washed with ethyl acetate and made alkaline with an aqueous solution of potassium carbonate. The resultant precipitates were collected by filtration, washed with water, dried and recrystallized from methanol and then from ethanol to give dark red crystals of 6-(4-chlorophenyl)-3-[2-(2-imidazolin-2-yl)hydrazino]-5-methyl-1,2,4-triazine (1.53 g), m.p. 230°~231° C. (decomp.).

Aufarbeitung

  1. temperaturewas refluxed for 3 hours
  2. temperatureAfter cooling
  3. customthe mixture was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in 1N hydrochloric acid
  5. washThe solution was washed with ethyl acetate
  6. customThe resultant precipitates
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customdried
  10. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-62ab3297fbc64afdbb932da8de2854f1
Quelldatensatz
uspto-grants-1986_10
Patentnummer
US04616014

Notizen zur Reaktion

Wird geladen…