Triethylamine → HCID 12671194, Verbindung

HRID 435976Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 435976
Cl[C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([CH3:11])[C:3]=1[CH2:12][CH2:13]Cl.Cl.[CH2:16]([NH2:20])[CH2:17][CH2:18][CH3:19].C(N(CC)CC)C>C(O)C>[CH2:16]([N:20]1[C:2]2[N:7]3[N:8]=[CH:9][N:10]=[C:6]3[N:5]=[C:4]([CH3:11])[C:3]=2[CH2:12][CH2:13]1)[CH2:17][CH2:18][CH3:19]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 36386487-chloro-6-(2-chloroethyl)-5-methyl[1,2,4]triazolo[1,5-a]pyrimidineHCID 64324001-Butanamine, hydrochloride (1:1)

Produkt 1

HCID 12671194HCID 12671194, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 2g of 7-chloro-6-(2-chloroethyl)-5-methyl-s-triazolo[1,5-a]pyrimidine, 0.95g of n-butylamine hydrochloride, 4 ml of triethylamine and 20 ml of ethanol was stirred under reflux for 1 hour. The reaction mixture was then concentrated under reduced pressure and the residue was dissolved in chloroform and purified by an column chromatography of alumina. The crystals thus obtained were recrystallized from isopropyl ether affording 1.35g of pale yellow needles of m.p. 72° - 75° C.

Aufarbeitung

  1. temperatureunder reflux for 1 hour
  2. concentrationThe reaction mixture was then concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in chloroform
  4. custompurified by an column chromatography of alumina
  5. customThe crystals thus obtained
  6. customwere recrystallized from isopropyl ether affording 1.35g of pale yellow needles of m.p. 72° - 75° C.

Quellen und Nachweise

ORD-Eintrag
ord-ef398a7d0cf74e24860472c66a5b7f2e
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04007189

Notizen zur Reaktion

Wird geladen…