Gamma-Butyrolactone → HCID 20340747, Verbindung

HRID 1395261Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1395261
[I-].[NH2:2][N+:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH2:9].[C:10]1(=O)[O:14][CH2:13][CH2:12][CH2:11]1.C(=O)([O-])[O-].[K+].[K+]>>[OH:14][CH2:13][CH2:12][CH2:11][C:10]1[N:9]=[C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][N:3]2[N:2]=1

Komponenten

4

Edukt 3

HCID 7302Gamma-ButyrolactoneHCID 11430Potassium CarbonateHCID 129098391,2-Diaminopyridinium iodide

Produkt 1

HCID 20340747HCID 20340747, Verbindung

Versuchsvorschrift

A mixture of 24 g of 1,2-diaminopyridinium iodide, 17.2 g of γ-butyrolactone and 57 g of potassium carbonate in 100 ml of diethylcellosolve was refluxed with stirring for 8 hours. The mixture was concentrated under reduced pressure to the residue, which was extracted by hot dichloromethane. The solvent was removed to give crude 2-(3-hydroxypropyl)-s-triazolo[1,5-a]pyridine, which was recrystallized from ethyl acetate to colorless needles (16 g, 90%), mp 71.5°-73° C. Anal. Calcd. for C9H11ON3 : C, 61.00; H, 6.24; N, 23.72. Found: C, 60.82; H, 6.14; N, 23.48.

Aufarbeitung

  1. temperaturewas refluxed
  2. concentrationThe mixture was concentrated under reduced pressure to the residue, which
  3. extractionwas extracted by hot dichloromethane
  4. customThe solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-88bfdba64b354e7999cf098a7ee5a1ba
Quelldatensatz
uspto-grants-1980_05
Patentnummer
US04202977

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