Triethylamine → HCID 19017552, Verbindung

HRID 1728318Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1728318
Cl[C:2]1[C:11]2[C:6](=[C:7]([F:12])[CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][N:3]=1.[F:13][C:14]([F:32])([F:31])[C:15]1[CH:16]=[CH:17][C:18]([O:21][C:22]2[CH:27]=[CH:26][C:25]([CH2:28][CH2:29][NH2:30])=[CH:24][CH:23]=2)=[N:19][CH:20]=1.C(N(CC)CC)C>C(O)C>[F:12][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:6]=1[N:5]=[CH:4][N:3]=[C:2]2[NH:30][CH2:29][CH2:28][C:25]1[CH:24]=[CH:23][C:22]([O:21][C:18]2[CH:17]=[CH:16][C:15]([C:14]([F:32])([F:13])[F:31])=[CH:20][N:19]=2)=[CH:27][CH:26]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 167707892-(4-(5-Trifluoromethyl-2-pyridinyloxy)phenyl)ethylamineHCID 199391334-Chloro-8-fluoroquinazoline

Produkt 1

HCID 19017552HCID 19017552, VerbindungAusbeute 58,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 4-chloro-8-fluoroquinazoline (1.82 g, 0.01 mol), 2-(4-(5-trifluoromethyl-2-pyridinyloxy)-phenyl)ethylamine (2.82 g, 0.01 mol), triethylamine (1.1 g, 0.011 mol) and ethanol (50 mL) was heated under reflux for three hours and allowed to cool. Solvent was evaporated under reduced pressure, and the residue dissolved in dichloromethane. This was washed with 0.5M sodium hydroxide solution and water, and dried over anhydrous sodium sulphate. Evaporation of the solvent under reduced pressure and recrystallization from ethyl acetate:hexane gave 2.5 g of product. MP 152° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for three hours
  3. temperatureto cool
  4. customSolvent was evaporated under reduced pressure
  5. dissolutionthe residue dissolved in dichloromethane
  6. washThis was washed with 0.5M sodium hydroxide solution and water
  7. dry with materialdried over anhydrous sodium sulphate
  8. customEvaporation of the solvent
  9. customunder reduced pressure and recrystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-2795b2e23daa46afa4c842df39bf5142
Quelldatensatz
uspto-grants-1994_07
Patentnummer
US05326766

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