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Triethylamine → HCID 178437548, Verbindung

HRID 1182894
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1182894
C(N(CC)CC)C.[C:8]([C@@H:12]1[CH2:17][CH2:16][C@H:15]([NH2:18])[CH2:14][CH2:13]1)([CH3:11])([CH3:10])[CH3:9].[CH2:19]([C:21]1[C:26]([Cl:27])=[C:25](Cl)[N:24]2[N:29]=[CH:30][N:31]=[C:23]2[N:22]=1)[CH3:20]>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[C:8]([C@@H:12]1[CH2:13][CH2:14][C@H:15]([NH:18][C:25]2[N:24]3[N:29]=[CH:30][N:31]=[C:23]3[N:22]=[C:21]([CH2:19][CH3:20])[C:26]=2[Cl:27])[CH2:16][CH2:17]1)([CH3:11])([CH3:9])[CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 860365485-Ethyl-6,7-dichloro-[1,2,4]triazolo[1,5-a]pyrimidineHCID 178445676HCID 178445676, Verbindung

Produkt 1

HCID 178437548HCID 178437548, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 67553Tetrabutylammonium IodideKatalysator
HCID 1140
Toluene
Lösungsmittel

Versuchsvorschrift

0.280 g (2.76 mmol) Triethylamine, a spatula tip of tetrabutylammonium iodide and 0.393 g (2.53 mmol) of cis-4-tert-butylcyclohexylamine were added successively to a solution of 0.500 g (2.3 mmol) of 5-ethyl-6,7-dichloro-[1,2,4]triazolo[1,5-a]pyrimidine in 10 ml of toluene under stirring. The reaction mixture was heated at reflux for 5 hours and then stirred for another 12 hours at room temperature. The solvent was evaporated under reduced pressure and dichloromethane was added to the resulting residue. The resulting reaction mixture was washed with 2N hydrochloric acid and water. The organic phase was separated, dried and the solvent was evaporated under reduced pressure. Treatment of the resulting residue with hexane yielded 0.420 g (1.2 mmol, 52% of theory) of the title compound having a melting point of 120-122° C.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 5 hours
  3. stirringstirred for another 12 hours at room temperature
  4. customThe solvent was evaporated under reduced pressure and dichloromethane
  5. additionwas added to the resulting residue
  6. customThe resulting reaction mixture
  7. washwas washed with 2N hydrochloric acid and water
  8. customThe organic phase was separated
  9. customdried
  10. customthe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9933950272ec41d683ebee04a9c65445
Quelldatensatz
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08664235B2

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