Hydrochloric Acid → HCID 178432390, Verbindung

HRID 1348549Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1348549
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[CH2:9][C:10](=O)[CH2:11]C(OCC)=O.[ClH:18].[NH2:19][C:20]1[NH:21][CH:22]=[CH:23][N:24]=1.[CH2:25]1CN2C(=NCCC2)C1.Cl.[OH2:35]>C(Cl)(Cl)Cl.CN(C)C=O>[OH:35][C:25]1[N:21]2[CH:22]=[CH:23][N:24]=[C:20]2[N:19]=[C:10]([CH3:11])[C:9]=1[C:3]1[C:4]([F:8])=[CH:5][CH:6]=[CH:7][C:2]=1[Cl:18]

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 962Water2×HCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 122112381H-Imidazol-2-amine hydrochlorideHCID 63022492Ethyl (2-chloro-6-fluorophenyl)acetoacetate

Produkt 1

HCID 178432390HCID 178432390, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 1.29 g of ethyl (2-chloro-6-fluorophenyl)acetoacetate, 0.60 g of aminoimidazole hydrochloride, 1.24 g of 1,5-diazabicyclo[4.3.0]-5-nonene (DBN) and 5 ml of N,N-dimethylformamide was heated at 100° C. for 14 hours. The reaction mixture was allowed to cool, and chloroform and water were added thereto. To the separated water layer, conc. hydrochloric acid was added and the precipitate was filtered, which was followed to subject to silica gel chromatography to give 0.16 g of 5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine.

Aufarbeitung

  1. temperatureto cool
  2. filtrationthe precipitate was filtered

Quellen und Nachweise

ORD-Eintrag
ord-7054545e715948659e3fcd2f805a7e49
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07211545B2

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