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Ethanol → HCID 14274201, Verbindung

HRID 1032003
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1032003
[CH3:1][S:2]([NH:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH:8]=[CH:9][CH:10]=[C:11]2[OH:16])(=[O:4])=[O:3].C(O)C.[N:20]([O-])=[O:21].[Na+]>O.[Cl-].[Zn+2].[Cl-]>[N:20]([C:10]1[CH:9]=[CH:8][C:7]2[C:12](=[CH:13][CH:14]=[CH:15][C:6]=2[NH:5][S:2]([CH3:1])(=[O:4])=[O:3])[C:11]=1[OH:16])=[O:21]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 702EthanolHCID 104704Methanesulfonamide, N-(5-hydroxy-1-naphthalenyl)-HCID 23668193Sodium Nitrite

Produkt 1

HCID 14274201HCID 14274201, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 962Water
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A mixture comprising 119 g of 5-methanesulfonylamino-1-naphthol, 100 g of zinc chloride and 500 ml of ethanol was heated at 50° C., and then a solution of 35 g of sodium nitrite as dissolved in 70 ml of water was added dropwise thereto at 50° to 65° C. After being heated and stirred at 60° to 65° C. for 2 hours, the resulting solution was cooled with water to room temperature, and reddish brown crystals formed were taken out by filtration and washed with ethanol. The crystals were added to 200 ml of concentrated hydrochloric acid and stirred for 1 hour at room temperature, and then 200 ml of water was added thereto. Yellowish brown crystals (2-nitroso-5-methanesulfonylamino-1-naphthol) formed were taken out by filtration, washed with water and dried. Yield: 90 g.

Aufarbeitung

  1. additionwas added dropwise
  2. customat 50° to 65° C
  3. temperatureAfter being heated
  4. customformed
  5. filtrationwere taken out by filtration
  6. washwashed with ethanol
  7. additionThe crystals were added to 200 ml of concentrated hydrochloric acid
  8. stirringstirred for 1 hour at room temperature
  9. addition200 ml of water was added

Quellen und Nachweise

ORD-Eintrag
ord-9abec76542314cb5849ae40ff6f0558d
Quelldatensatz
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04956456

Notizen zur Reaktion

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