N-bromobutanimide → HCID 67125220, Verbindung

HRID 874184Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 874184
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][N:11]=[C:10]([CH3:19])[N:9]=1.[Br:20]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:20][CH2:19][C:10]1[N:9]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][N:11]=1

Komponenten

4

Edukt 2

HCID 67184N-bromobutanimideHCID 18981952Ethyl 4-(2-chlorophenyl)-2-methylpyrimidine-5-carboxylate

Produkt 1

HCID 67125220HCID 67125220, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

820 mg (2.96 mmol) of ethyl 4-(2-chlorophenyl)-2-methylpyrimidine-5-carboxylate and 633 mg (3.55 mmol) of N-bromosuccinimide were dissolved in 18 ml of carbon tetrachloride and, with stirring, heated to the boil. At boiling point, 49 mg (0.29 mmol) of 2,2′-azobis-2-methylpropionitrile were added a little at a time over a period of 5 hours, followed by refluxing for a further hour. After cooling to room temperature, the reaction solution was filtered and the mother liquor was freed from the solvent under reduced pressure. The desired product was isolated by chromatographic purification.

Aufarbeitung

  1. temperatureheated to the boil
  2. additionwere added a little at a time over a period of 5 hours
  3. temperatureby refluxing for a further hour
  4. filtrationthe reaction solution was filtered

Quellen und Nachweise

ORD-Eintrag
ord-f560c7d869f14d1fb147ae7209bc58bf
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08980886B2

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