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2-Nitropropane → HCID 12621362, Verbindung

HRID 1730155
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1730155
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13](=[O:22])[CH:14]=[CH:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[N+:23]([CH:26]([CH3:28])[CH3:27])([O-:25])=[O:24].C(O)C.CC[O-].[Na+]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13](=[O:22])[CH2:14][CH:15]([C:16]2[CH:17]=[CH:18][N:19]=[CH:20][CH:21]=2)[C:26]([CH3:28])([N+:23]([O-:25])=[O:24])[CH3:27])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 3982-NitropropaneHCID 702EthanolHCID 2723922Sodium ethoxideHCID 540288583-(Pyridin-4-yl)-1-(3,4,5-trimethoxyphenyl)prop-2-en-1-one

Produkt 1

HCID 12621362HCID 12621362, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel

Versuchsvorschrift

A solution of 40 g. of 3',4',5'-trimethoxy-3-(4-pyridyl)-acrylophenone and 24 g. of 2-nitropropane in 270 ml. of ethanol is heated at reflux with stirring under a nitrogen atmosphere. Within 1 hour there is added dropwise a sodium ethylate solution (manufactured from 1.35 g. of sodium and 27 ml. of ethanol). The reaction mixture left standing for a half hour to react further is then evaporated under reduced pressure. The residue results is taken up in methylene chloride, washed with water, dried over sodium sulfate and evaporated under reduced pressure. The product which results is crystallized with chloroform ether to yield 3',4',5'-trimethoxy-4-methyl-4-nitro-3-(4-pyridyl)-valerophenone, melting point 214°-216° C.

Aufarbeitung

  1. temperatureat reflux
  2. waitThe reaction mixture left
  3. waitstanding for a half hour
  4. customto react further
  5. customis then evaporated under reduced pressure
  6. customThe residue results
  7. washwashed with water
  8. dry with materialdried over sodium sulfate
  9. customevaporated under reduced pressure
  10. customThe product which results
  11. customis crystallized with chloroform ether

Quellen und Nachweise

ORD-Eintrag
ord-86da33ee5be4429697b5679ec2ee1fd7
Quelldatensatz
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03991197

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