Tributylamine → HCID 178432402, Verbindung

HRID 1986636Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1986636
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.[CH:7]1([CH:12]([C:18](=O)[CH3:19])[C:13](OCC)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8]1.C(N(CCCC)CCCC)CCC>[OH-].[Na+]>[CH3:19][C:18]1[C:12]([CH:7]2[CH2:11][CH2:10][CH2:9][CH2:8]2)=[C:13]([OH:14])[N:3]2[N:4]=[CH:5][N:6]=[C:2]2[N:1]=1

Komponenten

5

Edukt 3

HCID 7622TributylamineHCID 17750296Ethyl 2-cyclopentyl-3-oxobutanoateHCID 178418311HCID 178418311, Verbindung

Produkt 1

HCID 178432402HCID 178432402, VerbindungAusbeute 52,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

A mixture of 3-amino-1,2,4-triazole (14 g), ethyl 2-cyclopentyl-3-oxobutanoate (0.17 mol, Ex. 1) and tributylamine (50 ml) was heated at 180° C. for 6 hours. The reaction mixture was cooled to about 70° C., and aqueous NaOH solution (21 g in 200 ml of H2O) was then added and the solution was stirred for another 30 min. Following phase separation and extraction with diethyl ether, the aqueous phase was acidified with conc. HCl solution. The precipitate gave 19 g of the title compound.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to about 70° C.
  2. customFollowing phase separation and extraction with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-57d71b38b94e4789b7f567a5272e2cb5
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07550471B2

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