Hydrochloric Acid → 6-Azidosulfonylhexyltriethoxysilane

HRID 1194067Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1194067
[N-:1]=[N+:2]=[N-:3].[Na+].Cl.[N-]=[N+]=[N-].[CH2:9]([O:11][Si:12]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][S:25](Cl)(=[O:27])=[O:26])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])[CH3:10]>P([O-])([O-])(O)=O.[Na+].[Na+].C(Cl)Cl>[CH2:9]([O:11][Si:12]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][S:25]([N:1]=[N+:2]=[N-:3])(=[O:27])=[O:26])([O:13][CH2:14][CH3:15])[O:16][CH2:17][CH3:18])[CH3:10]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 33558AzideHCID 86742803HCID 86742803, Verbindung

Produkt 1

HCID 220457406-Azidosulfonylhexyltriethoxysilane

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 24203Sodium Phosphate, DibasicLösungsmittel

Versuchsvorschrift

Sodium azide (1.5 equivalent) in 4 ml of sodium hydrogen phosphate and hydrogen chloride buffer (14.4 g or Na2HPO4 to 4.4 mil conc HCl in 1 liter of distilled water) per gram of azide is added dropwise to a stirred 50 percent solution of triethoxysilylhexane sulfonyl chloride in methylene chloride containing 1 percent Aliquat 336. The mixture is stirred at room temperature for thirty minutes after the addition is complete. The layers are separated. The methylene chloride layer is washed with a saturated salt solution, dried over magnesium sulfate and the methylene chloride is evaporated. Ninety percent solids of a light yellow liquid triethoxysilylhexane sulfonyl azide of about 90 percent purity are obtained.

Aufarbeitung

  1. additionafter the addition
  2. customThe layers are separated
  3. washThe methylene chloride layer is washed with a saturated salt solution
  4. dry with materialdried over magnesium sulfate
  5. customthe methylene chloride is evaporated

Quellen und Nachweise

ORD-Eintrag
ord-9787aeaaecd34093a042e510810e6d2c
Quelldatensatz
uspto-grants-1989_03
Patentnummer
US04812519

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