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Triethylamine → HCID 57519920, Verbindung

HRID 1528096
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1528096
ClC(O[C:6](=[O:12])OC(Cl)(Cl)Cl)(Cl)Cl.[F:13][C:14]([F:23])([F:22])[C:15]1[N:20]=[C:19]([NH2:21])[CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.[Br:31][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][CH:36]=[C:35]2[NH2:42]>ClCCl>[Br:31][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][CH:36]=[C:35]2[NH:42][C:6]([NH:21][C:19]1[CH:18]=[CH:17][CH:16]=[C:15]([C:14]([F:13])([F:22])[F:23])[N:20]=1)=[O:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471Triethylamine2×HCID 94429TriphosgeneHCID 8210242-Amino-6-(trifluoromethyl)pyridineHCID 27563746-Bromoquinolin-4-amine

Produkt 1

HCID 57519920HCID 57519920, VerbindungAusbeute 159,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel
3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

366 mg of bis(trichloromethyl)carbonate (1.234 mmol) were dissolved in 7 ml of dichloromethane (DCM) and cooled to 0° C. To this mixture a solution of 400 mg 6-(trifluoromethyl)pyridin-2-amine (2.467 mmol) and 379 μl triethylamine (5.43 mmol) in 9.7 ml DCM was slowly added over 60 minutes at 0° C. and stirring was then continued for additional 60 minutes at 23° C. 550 mg 6-bromoquinolin-4-amine (2.467 mmol) and 379 μl triethylamine (5.43 mmol) were suspended in 9.7 ml DCM and the suspension was slowly added to the reaction mixture at 23° C., which became a clear solution after 45 minutes. After stirring over night the reaction mixture was poured into ice water and stirred for 2 h. The precipitate formed was filtered off and dried in vacuo for 24 h. 810 mg of the desired product were obtained as off white powder (yield: 80%). The already quite pure raw material was used without further purification.

Aufarbeitung

  1. additionthe suspension was slowly added to the reaction mixture at 23° C.
  2. customafter 45 minutes
  3. stirringAfter stirring over night the reaction mixture
  4. stirringstirred for 2 h
  5. customThe precipitate formed
  6. filtrationwas filtered off
  7. customdried in vacuo for 24 h

Quellen und Nachweise

ORD-Eintrag
ord-873d9ed060974ecdb92d825c704d8127
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09090592B2

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