Triethanolamine → Tris-(2-hydroxyethyl)ammonium 5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrobenzoate

HRID 65333

Reaktionsgleichung

Reaktionsgleichung von HRID 65333
[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:14]([O-:16])=[O:15])=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11].[N:25]([CH2:32][CH2:33][OH:34])([CH2:29][CH2:30][OH:31])[CH2:26][CH2:27][OH:28]>C(COC)OC>[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:22])([F:23])[F:24])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:14]([O-:16])=[O:15])=[C:9]([CH:13]=1)[C:10]([O-:12])=[O:11].[OH:28][CH2:27][CH2:26][NH+:25]([CH2:32][CH2:33][OH:34])[CH2:29][CH2:30][OH:31]

Komponenten

4

Versuchsvorschrift

5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrobenzoic acid (3.0 g, 0.0083 mole) is dissolved in glyme (20 ml) and a solution of triethanolamine (1.35 g, 0.0091 mole) in glyme (5 ml) is added rapidly while stirring at room temperature. After stirring for a few hours the solvent is removed in vacuo, the product is triturated repeatedly with petroleum ether (bp 30°-60° C.) and dried to a weight of 2.5 g. Anal. Calcd. for C20H22ClF3N2O8 : C, 47.02; H, 4.34; Cl, 6.39; N, 5.48; F, 11.15. Found: C, 47.08; H, 4.78; Cl, 6.48; N, 5.21; F, 10.16.

Aufarbeitung

  1. stirringAfter stirring for a few hours the solvent
  2. customis removed in vacuo
  3. customthe product is triturated repeatedly with petroleum ether (bp 30°-60° C.)
  4. customdried to a weight of 2.5 g

Quellen und Nachweise

ORD-Eintrag
ord-0c52bc6e3fed4a899dc35356e0f09206
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04613360

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