반응 #93611

ord-0c52bc6e3fed4a899dc35356e0f09206

반응 방정식

O=C(O)c1cc(Oc2ccc(C(F)(F)F)cc2Cl)ccc1[N+](=O)[O-]
5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrobenzoic acid
OCCN(CCO)CCO
triethanolamine
O=C([O-])c1cc(Oc2ccc(C(F)(F)F)cc2Cl)ccc1[N+](=O)[O-].OCC[NH+](CCO)CCO
Tris-(2-hydroxyethyl)ammonium 5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrobenzoate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGAfter stirring for a few hours the solvent
  2. 2
    기타is removed in vacuo
  3. 3
    기타the product is triturated repeatedly with petroleum ether (bp 30°-60° C.)
  4. 4
    기타dried to a weight of 2.5 g

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04613360uspto-grants-1986_09