Water → 2-[4'-(4"-Chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester

HRID 903380Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 903380
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[C:13]([OH:15])=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[Cl:21][CH2:22][CH2:23][CH2:24][CH2:25]O.S(=O)(=O)(O)O.O>C(Cl)(Cl)Cl>[Cl:21][CH2:22][CH2:23][CH2:24][CH2:25][O:14][C:13](=[O:15])[CH:12]([O:11][C:10]1[CH:17]=[CH:18][C:7]([O:6][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:20][CH:19]=2)=[CH:8][CH:9]=1)[CH3:16]

Komponenten

6

Edukt 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 135694-Chloro-1-butanolHCID 64928Clofop

Produkt 1

HCID 544272872-[4'-(4"-Chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

24.4 g=0.08 mol of 2-[4'-(4"-chlorophenoxy)phenoxy]-propionic acid, 10.8 g=0.1 mol of 4-chlorobutanol and 2 ml concentrated sulfuric acid in 50 ml chloroform were refluxed for 6 hours with azeotropic distillation of the reaction water. After cooling, the reaction mixture was washed twice with 100 ml water, neutralized with bicarbonate solution and washed with water until it was free from salt. After drying over calcium chloride and distillation of the solvent, 27.0 g=88% of the theory of 2-[4'-(4"-chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester were obtained having a refractive index nD24 of 1.5517. ##STR16##

Aufarbeitung

  1. temperatureAfter cooling
  2. washthe reaction mixture was washed twice with 100 ml water
  3. washwashed with water until it
  4. dry with materialAfter drying over calcium chloride and distillation of the solvent, 27.0 g=88% of the theory of 2-[4'-(4"-chlorophenoxy)phenoxy]-propionic acid 4-chlorobut-1-yl ester
  5. customwere obtained

Quellen und Nachweise

ORD-Eintrag
ord-9eea7b03f4744be98d8b812d6cfd0338
Quelldatensatz
uspto-grants-1980_10
Patentnummer
US04227009

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