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Thionyl Chloride → trans 3-Bromocinnamoyl chloride

HRID 372477
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 372477
[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7](O)=[O:8].S(Cl)([Cl:15])=O>C1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7]([Cl:15])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24386Thionyl Chloride2×HCID 776461m-Bromocinnamic acid

Produkt 1

HCID 14959106trans 3-Bromocinnamoyl chlorideAusbeute 99,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

Trans m-bromocinnamic acid (11.4 g) in dry benzene (75 ml) was heated to reflux and then a mixture of thionyl chloride (12 g) in dry benzene (50 ml) was added at such a rate as to maintain constant reflux. The reaction mixture was heated at reflux for an additional 2 hr after the addition of thionyl chloride. The solvent and excess thionyl chloride were then removed under reduced pressure to give trans 3-bromocinnamoyl chloride (ca. 12.3 g). A solution of the 3-bromocinnamoyl chloride in toluene (150 ml) was added dropwise with stirring to a solution of isopropylamine (10 g) in ether (200 ml). The reaction mixture was stirred at room temperature for one hour and then heated at reflux for one hour. The solvent and excess amine were removed under reduced pressure. The crude residue was triturated with water, filtered, and recrystallized from ethanol-water to give white, crystalline trans 3-bromo-N-isopropylcinnamamide, m.p. 85°-86° C. Elemental analysis, NMR and IR spectra all confirmed the identity of the product.

Aufarbeitung

  1. temperatureto reflux
  2. additionwas added at such a rate as
  3. temperatureto maintain constant reflux
  4. temperatureThe reaction mixture was heated
  5. temperatureat reflux for an additional 2 hr
  6. customThe solvent and excess thionyl chloride were then removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1602dc8d2a8c4baa8ab8a88a0ae28d29
Quelldatensatz
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04091112

Notizen zur Reaktion

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