Acetone → HCID 13657069, Verbindung

HRID 745674

Reaktionsgleichung

Reaktionsgleichung von HRID 745674
[Cl:1][C:2]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:13]([O-:15])=[O:14])=[C:9]([CH:12]=1)[CH2:10]Cl.[C:24]([O:34][CH2:35][CH3:36])(=[O:33])[CH:25]([CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])[OH:26].C(N(CC)CC)C.CC(C)=[O:46]>O>[CH2:35]([O:34][C:24]([CH:25]([O:26][C:10](=[O:46])[C:9]1[CH:12]=[C:5]([O:4][C:3]2[CH:16]=[CH:17][C:18]([C:20]([F:23])([F:22])[F:21])=[CH:19][C:2]=2[Cl:1])[CH:6]=[CH:7][C:8]=1[N+:13]([O-:15])=[O:14])[CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:33])[CH3:36]

Komponenten

6

Edukt 4

HCID 180Acetone3×HCID 8471TriethylamineHCID 24197Diethyl malateHCID 13090781HCID 13090781, Verbindung

Produkt 1

HCID 13657069HCID 13657069, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzyl chloride (3.8 g, 0.01 mole) in acetone (10 ml) was successively added diethyl DL malate (1.9 g, 0.01 mole) in acetone (10 ml) and triethylamine (1.01 g, 0.01 mole) in acetone (5 ml). A white precipitate quickly formed. The reaction was heated to reflux for 24 hours. Upon cooling, the reaction was poured in water (75 ml) and extracted twice with methylene chloride (25 ml@). The combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions. The dried solution was stripped of solvent to give 3.5 g of an amber oil.

Aufarbeitung

  1. customA white precipitate quickly formed
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 24 hours
  4. temperatureUpon cooling
  5. extractionextracted twice with methylene chloride (25 ml@)
  6. washThe combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions

Quellen und Nachweise

ORD-Eintrag
ord-b14a83937ea54b66b9bb63b80b93e972
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04599442

Verknüpfte Notizen

Wird geladen…