2-[(2-chloro-1-oxo-propyl)-amino]-beta-oxo-N-(2-pyridinyl)-3-trifluoromethyl-benzene-propanamide → HCID 178434920, Verbindung

HRID 1982597Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1982597
Cl[CH:2]([CH3:28])[C:3]([NH:5][C:6]1[C:11]([C:12]([F:15])([F:14])[F:13])=[CH:10][CH:9]=[CH:8][C:7]=1[C:16](=[O:27])[CH2:17][C:18]([NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1)=[O:19])=O>CN(C)C1C=CN=CC=1.O1CCCC1>[CH3:28][CH:2]1[C:3]2=[N:5][C:6]3[C:11]([C:12]([F:14])([F:15])[F:13])=[CH:10][CH:9]=[CH:8][C:7]=3[C:16]([OH:27])=[C:17]2[C:18](=[N:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=2)[O:19]1

Komponenten

4

Edukt 1

HCID 134231002-[(2-chloro-1-oxo-propyl)-amino]-beta-oxo-N-(2-pyridinyl)-3-trifluoromethyl-benzene-propanamide

Produkt 1

HCID 178434920HCID 178434920, VerbindungAusbeute 115,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

1.60 g of 4-dimethylamino-pyridine were added to a suspension of 4.5 g of the product of Step A in 90 ml of tetrahydrofuran and the mixture was refluxed for four hours and was evaporated to dryness under reduced pressure. The residue was added to 90 ml of water and the mixture was stirred for 30 minutes and was vacuum filtered. The product was washed with water and dried under reduced pressure at 70° C. to obtain 4.50 g of 1,3-dihydro-3-methyl-1-[(2-pyridinyl)-imino]-5-trifluoromethyl-furo[3,4-b]quinoline-9-ol which was crystallized from absolute ethanol.

Aufarbeitung

  1. temperaturethe mixture was refluxed for four hours
  2. customwas evaporated to dryness under reduced pressure
  3. additionThe residue was added to 90 ml of water
  4. filtrationfiltered
  5. washThe product was washed with water
  6. customdried under reduced pressure at 70° C.

Quellen und Nachweise

ORD-Eintrag
ord-aa214c477d5b47a78aad155f58d60461
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04596875

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