Ethanol → HCID 178470502, Verbindung

HRID 485386

Reaktionsgleichung

Reaktionsgleichung von HRID 485386
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[N:3]=1.[N:11]1([CH2:17][C:18]2[CH:19]=[C:20]([CH:27]=[CH:28][CH:29]=2)[O:21][CH2:22][CH2:23][CH2:24][CH:25]=O)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.[BH4-].[Na+].[CH2:32](O)C>>[N:11]1([CH2:17][C:18]2[CH:19]=[C:20]([CH:27]=[CH:28][CH:29]=2)[O:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:1][C:2]2[NH:6][N:5]=[C:4]([C:7]([O:9][CH2:10][CH3:32])=[O:8])[N:3]=2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1

Komponenten

5

Edukt 4

HCID 702EthanolHCID 4311764Sodium borohydrideHCID 212975474-[3-(1-Piperidinylmethyl)phenoxy]butanalHCID 178499187HCID 178499187, Verbindung

Produkt 1

HCID 178470502HCID 178470502, Verbindung

Versuchsvorschrift

Methyl 5-amino-1H-1,2,4-triazole-3-carboxylate (0.568 g) and 4-[3-(1-piperidinylmethyl)phenoxy]butanal in ethanol (40 ml) were heated at reflux for 2 h. The cooled reaction mixture was treated with sodium borohydride (0.4 g) and stirred at room temperature for 15 h. The solvent was evaporated and the residue was dissolved in 2N hydrochloric acid which was washed with ethyl acetate, basified with sodium carbonate and extracted with ethyl acetate. The combined organic extracts were evaporated to yield the title compound as a white solid which was recrystallised from a mixture of ethyl acetate and ethanol (1:1) (0.5 g) m.p. 170°-1° dec.; tlc System B, Rf 0.8.

Aufarbeitung

  1. temperatureat reflux for 2 h
  2. customThe cooled reaction mixture
  3. customThe solvent was evaporated
  4. dissolutionthe residue was dissolved in 2N hydrochloric acid which
  5. washwas washed with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. customThe combined organic extracts were evaporated

Quellen und Nachweise

ORD-Eintrag
ord-32393270926f4dd58ed3dd761f6622d0
Quelldatensatz
uspto-grants-1985_08
Patentnummer
US04536508

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