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Hydrochloric Acid → HCID 178434075, Verbindung

HRID 461587
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 461587
[CH3:1][N:2]1[C:6](=[O:7])[CH:5]=[C:4]([CH3:8])[NH:3]1.[OH-].[Ca+2].[OH-].[N+:12]([C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=1)([O-:14])=[O:13].Cl>O1CCOCC1>[CH3:1][N:2]1[C:6]([OH:7])=[C:5]([C:19](=[O:20])[C:18]2[CH:17]=[CH:16][C:15]([N+:12]([O-:14])=[O:13])=[CH:23][CH:22]=2)[C:4]([CH3:8])=[N:3]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 85024-Nitrobenzoyl chlorideHCID 27668471,3-dimethyl-1H-pyrazol-5-olHCID 6093208Calcium Hydroxide

Produkt 1

HCID 178434075HCID 178434075, VerbindungAusbeute 69,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31275
1,4-Dioxane
Lösungsmittel

Versuchsvorschrift

In 22 ml. of dry dioxane is dissolved 2.24 g. of 1,3-dimethyl-5-pyrazolone and then 2.96 g. of calcium hydroxide is added thereto. 3.71 g. of p-nitrobenzoyl chloride is added dropwise thereto while stirring at room temperature. After completion of the dropwise addition, the mixture is heated under reflux for 1 hour. After completion of the reaction, the reaction mixture is allowed to cool and then 40 ml. of a 2N hydrochloric acid solution is added thereto. Crystalline substances thus separated are recovered by filtration and washed with water to give 4.38 g. of crude crystals. This product is recrystallized from methanol to give 3.62 g. of the desired product as pale yellow columns having a melting point of 234°-235° C. Yield 69.3%

Aufarbeitung

  1. additionAfter completion of the dropwise addition
  2. temperaturethe mixture is heated
  3. temperatureunder reflux for 1 hour
  4. customAfter completion of the reaction
  5. temperatureto cool
  6. customCrystalline substances thus separated
  7. filtrationare recovered by filtration
  8. washwashed with water
  9. customto give 4.38 g
  10. customThis product is recrystallized from methanol
  11. customto give 3.62 g

Quellen und Nachweise

ORD-Eintrag
ord-fdd6e5965c864d618a1716d2eb91aedb
Quelldatensatz
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04063925

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