Water → 2-[p-(2,4-Dichlorobenzyl)-phenoxi]-propionic acid amide

HRID 371890

Reaktionsgleichung

Reaktionsgleichung von HRID 371890
[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.Br[CH:18]([CH3:22])[C:19]([NH2:21])=[O:20].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[CH2:4][C:5]1[CH:6]=[CH:7][C:8]([O:11][CH:18]([CH3:22])[C:19]([NH2:21])=[O:20])=[CH:9][CH:10]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1011182-BromopropanamideHCID 139387094-(2,4-Dichlorobenzyl)-phenol

Produkt 1

HCID 706227402-[p-(2,4-Dichlorobenzyl)-phenoxi]-propionic acid amide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 25.3 g of 4-(2,4-dichlorobenzyl)-phenol and 15.2 g of α-bromopropionic acid amide in 100 ml of dimethyl formamide was stirred for 2 hours at 100° C together with 16 g of potassium carbonate. After cooling, the reaction mixture was poured into 1 liter of water. A viscous oil precipitated which was absorbed in methylene chloride and washed with water. After drying over sodium sulfate, the solvent was distilled off under reduced pressure. The remaining colorless crystals were recrystallized from methanol. Yield: 25.8 g; melting point 148° - 149° C. ##STR5##

Aufarbeitung

  1. temperatureAfter cooling
  2. customA viscous oil precipitated which
  3. customwas absorbed in methylene chloride
  4. washwashed with water
  5. dry with materialAfter drying over sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe remaining colorless crystals were recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-5991b704c0034b9283fb1896623af89d
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04088474

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