Hydrochloric Acid → HCID 178515569, Verbindung

HRID 727737Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 727737
[OH-].[Na+].Cl.[NH2:4]O.[C:6]([CH2:14][C:15]([O:17]CC)=O)(=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl>O.C(O)C>[C:7]1([C:6]2[O:13][N:4]=[C:15]([OH:17])[CH:14]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 7170Ethyl benzoylacetateHCID 14798Sodium Hydroxide3×HCID 443297Hydroxyamine hydrochloride

Produkt 1

HCID 178515569HCID 178515569, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel4×HCID 962WaterLösungsmittel4×

Versuchsvorschrift

40 g of sodium hydroxide was dissolved in 200 ml of water and 300 ml of ethanol. 69.5 g of hydroxylamine hydrochloride was added to the solution. A mixed solution of 2N sodium hydroxide and a 3:2 mixture of ethanol and water was added to the solution so that the pH thereof was adjusted to 10.0. 192 g of ethyl benzoylacetate and a mixed solution of 2N sodium hydroxide and a 3:2 mixture of ethanol and water were added dropwise to the solution at the same time under cooling with ice in such a manner that the pH thereof was 10±0.3. After the dropwise addition was finished, the solution was stirred at room temperature for 3 hours. The reaction mixture was then poured into a mixture of 500 g of conc. hydrochloric acid and 500 g of ice. 2.5 l of ethanol was added to the reaction mixture. The reaction mixture was heated under reflux for 3 hours. 2 l of water was added to cool the solution. The resulting crystals were filtered off, washed with water, and dried. (Yield: 98 g (61%); m.p.: 150°-151° C.)

Aufarbeitung

  1. additionwas added to the solution so that the pH
  2. additionwere added dropwise to the solution at the same time
  3. temperatureunder cooling with ice in such a manner that the pH
  4. additionAfter the dropwise addition
  5. temperatureThe reaction mixture was heated
  6. temperatureunder reflux for 3 hours
  7. temperatureto cool the solution
  8. filtrationThe resulting crystals were filtered off
  9. washwashed with water
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b76acdde1f89430a9ee8579d4b9280c0
Quelldatensatz
uspto-grants-1991_09
Patentnummer
USH0000963

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