N-bromobutanimide → HCID 67125220, Verbindung

HRID 1958084Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1958084
[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

An amount of 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 heated with stirring to boiling. At the heat of boiling, in portions, 49 mg (0.29 mmol) of 2,2′-azobis-2-methylpropanenitrile were added over 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
  2. temperatureAt the heat
  3. additionwere added over 5 hours
  4. temperatureby refluxing for a further hour
  5. filtrationthe reaction solution was filtered

Quellen und Nachweise

ORD-Eintrag
ord-cc4bbd6aafed4497bed39242722ecd9e
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08410106B2

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