Hydrochloric Acid → 2-Chloroethyl 2-[(3-nitrophenyl)methylidene]-3-oxobutanoate

HRID 1284913Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1284913
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=O)([O-:3])=[O:2].[C:12]([O:18][CH2:19][CH2:20][Cl:21])(=[O:17])[CH2:13][C:14]([CH3:16])=[O:15].Cl>C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=[C:13]([C:14]([CH3:16])=[O:15])[C:12]([O:18][CH2:19][CH2:20][Cl:21])=[O:17])([O-:3])=[O:2]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 74493-NitrobenzaldehydeHCID 108605Butanoic acid, 3-oxo-, 2-chloroethyl ester

Produkt 1

HCID 540552132-Chloroethyl 2-[(3-nitrophenyl)methylidene]-3-oxobutanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

10 Grams of 3-nitrobenzaldehyde and 11 g of 2-chloroethyl acetoacetate were dissolved in 100 ml of toluene, then under an ice-cooled condition, hydrogen chloride gas was introduced into the solution for 2 hours. The reaction mixture was allowed to stand at room temperature for 2 days, and was concentrated. The residue obtained was extracted with chloroform, then the chloroform layer was washed with a saturated sodium chloride aqueous solution and with a saturated sodium hydrogen carbonate aqueous solution and dried with anhydrous magnesium sulfate. Chloroform was removed by distillation and the residue was recrystallized from isopropanol to yield 10 g of 2-chloroethyl 2-(3-nitrobenzyliden)acetoacetate in the form of colorless needle-like crystals.

Aufarbeitung

  1. additionwas introduced into the solution for 2 hours
  2. concentrationwas concentrated
  3. customThe residue obtained
  4. extractionwas extracted with chloroform
  5. washthe chloroform layer was washed with a saturated sodium chloride aqueous solution and with a saturated sodium hydrogen carbonate aqueous solution
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customChloroform was removed by distillation
  8. customthe residue was recrystallized from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-ae2f417460a2403c8bbc65fb5b23a000
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04564619

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