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Thionyl Chloride → 4-(Chlorocarbonyl)phenyl benzoate

HRID 854223
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 854223
[C:1]([O:9][C:10]1[CH:18]=[CH:17][C:13]([C:14](O)=[O:15])=[CH:12][CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:21])=O>CN(C)C=O>[C:1]([O:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([Cl:21])=[O:15])=[CH:12][CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 119979Benzoic acid, 4-(benzoyloxy)-

Produkt 1

HCID 150272094-(Chlorocarbonyl)phenyl benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideKatalysator

Versuchsvorschrift

10.00 g (41.3 mmol) of 4-(benzoyloxy)benzoic acid and one drop of N,N-dimethylformamide are refluxed in 40 ml of thionyl chloride with stirring until gas is no longer evolved. The excess thionyl chloride is very substantially removed by distillation under reduced pressure and co-distilled twice with petroleum ether (50/70) under reduced pressure from the remaining residue for complete removal. Purification is carried out by recrystallization from 150 ml of petroleum ether (50/70)/ethyl acetate 2:1, and the crystals are washed with 4 ml of petroleum ether (50/70)

Aufarbeitung

  1. customThe excess thionyl chloride is very substantially removed by distillation under reduced pressure
  2. customco-distilled twice with petroleum ether (50/70) under reduced pressure from the remaining residue for complete removal
  3. customPurification
  4. customis carried out by recrystallization from 150 ml of petroleum ether (50/70)/ethyl acetate 2:1
  5. washthe crystals are washed with 4 ml of petroleum ether (50/70)

Quellen und Nachweise

ORD-Eintrag
ord-c5bb76b319364229ad4cf68f04c53584
Quelldatensatz
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07258902B2

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