Ammonium Hydroxide → HCID 178516142, Verbindung

HRID 1681199Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1681199
[F:1][C:2]([F:16])([F:15])[C:3](=O)[CH2:4][C:5](=[O:13])[CH2:6][C:7]([C:9]([F:12])([F:11])[F:10])=O.[OH-].[NH4+:18]>>[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([OH:13])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[N:18]=1

Komponenten

3

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of 30 g 1,5-di(trifluoromethyl)-1,3,5-trioxopentane and 125 ml 28% aqueous ammonium hydroxide was heated in an autoclave at 130° C. for 5 hours. The reaction mixture was concentrated in vacuo, dissolved in 350 ml ethanol and treated with 11 ml 6N hydrochloric acid. The resulting mixture was concentrated in vacuo, 100 ml water added to the residue and filtered to give 8.0 g 2,6-di(trifluoromethyl)-4-hydroxypyridine, m.p. 123°-130° C.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutiondissolved in 350 ml ethanol
  3. additiontreated with 11 ml 6N hydrochloric acid
  4. concentrationThe resulting mixture was concentrated in vacuo, 100 ml water
  5. additionadded to the residue
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-dec5f2061bb746b79ca7ef18cd3eadc1
Quelldatensatz
uspto-grants-1992_12
Patentnummer
US05169853

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