Methanol → 4-(4-n-Hexylpyrimid-2-yl)benzoic acid amide

HRID 461310Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 461310
Cl.[C:2]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([NH2:11])=[O:10])=[CH:7][CH:6]=1)(=[NH:4])[NH2:3].[CH2:14]([C:20](=[CH:23]OCC)C=O)[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].[CH3:27][O-].[Na+].CO>CCOCC>[CH2:15]([C:14]1[CH:20]=[CH:23][N:3]=[C:2]([C:5]2[CH:13]=[CH:12][C:8]([C:9]([NH2:11])=[O:10])=[CH:7][CH:6]=2)[N:4]=1)[CH2:16][CH2:17][CH2:18][CH2:19][CH3:27]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 27242934-Amidinobenzamide HydrochlorideHCID 10942334Sodium MethoxideHCID 542364922-n-Hexyl-3-ethoxy-acrolein

Produkt 1

HCID 541836714-(4-n-Hexylpyrimid-2-yl)benzoic acid amide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

0.082 mol of 4-amidino-benzoic acid amide hydrochloride, suspended in a solution of 0.082 mol of 2-n-hexyl-3-ethoxy-acrolein and 0.14 mol of sodium methylate in 150 ml. of methanol, are stirred overnight at room temperature under an atmosphere of nitrogen. The precipitate obtained by diluting the reaction mixture with 3.1 of ether is removed by filtration, washed with water until neutral and dried at 40° in a vacuum drying cabinet, whereby 17.9 g. of 4-(4-n-hexylpyrimid-2-yl)benzoic acid amide are obtained, m.p. 231.6° - 233.0°.

Aufarbeitung

  1. customThe precipitate obtained
  2. customis removed by filtration
  3. washwashed with water until neutral and
  4. customdried at 40° in a vacuum
  5. customdrying cabinet, whereby 17.9 g

Quellen und Nachweise

ORD-Eintrag
ord-2384ed2869fd4d3cb928e419bf92b052
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04062798

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