Water → HCID 20300028, Verbindung

HRID 1733698Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1733698
[OH:1][N:2]1[C:6]2[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=2[N:4]=[N:3]1.[C:14]1([S:20](Cl)(=[O:22])=[O:21])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.O.C(OCC)(=O)C>[OH-].[Na+]>[C:14]1([S:20]([O:1][N:2]2[C:6]3[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=3[N:4]=[N:3]2)(=[O:22])=[O:21])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 7369Benzenesulfonyl chlorideHCID 8857Ethyl AcetateHCID 1528171-Hydroxy-6-nitrobenzotriazole

Produkt 1

HCID 20300028HCID 20300028, VerbindungAusbeute 53,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

In 1 N aqueous sodium hydroxide (45 ml) is dissolved 1-hydroxy-6-nitro-1,2,3-benzotriazole (7.2 g). To the solution is added dropwise benzenesulfonyl chloride (7.0 g) with stirring at room temperature and further are added thereto water (50 ml) and ethyl acetate (100 ml) and the mixture is stirred for 1 hour. The ethyl acetate layer is separated, dried over magnesium sulfate-charcoal, filtered and concentrated until it becomes about 30 ml. n-Hexane (50 ml) is thereto added and the mixture is allowed to stand. The precipitated crystals are separated by filtration and dried to give faint yellow prisms of 1-benzenesulfonyloxy-6-nitro-1,2,3-benzotriazole (6.8 g), melting point: 122°-124° C. The product is recrystallized from ethyl acetate-n-hexane to give a pure product: melting point: 124° C.

Aufarbeitung

  1. additionfurther are added
  2. customThe ethyl acetate layer is separated
  3. dry with materialdried over magnesium sulfate-charcoal
  4. filtrationfiltered
  5. concentrationconcentrated until it
  6. additionn-Hexane (50 ml) is thereto added
  7. customThe precipitated crystals are separated by filtration
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e99f9d1d4a5d4ee4bb83db65fa9f4ce8
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04242507

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