Sodium Azide → HCID 23044225, Verbindung

HRID 2165159Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2165159
[N-:1]=[N+:2]=[N-:3].[Na+].[CH3:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH2:11][CH2:12][CH:13]([CH2:17]OS(C3C=CC(C)=CC=3)(=O)=O)[CH2:14]2)=[CH:9][CH:8]=1>O.C(O)C>[CH3:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH2:11][CH2:12][CH:13]([CH2:17][N:1]=[N+:2]=[N-:3])[CH2:14]2)=[CH:9][CH:8]=1

Komponenten

5

Edukt 2

HCID 33557Sodium AzideHCID 11210176p-Toluenesulphonic acid (7-methoxy-1,2,3,4-tetrahydro-naphth-2-ylmethyl) ester

Produkt 1

HCID 23044225HCID 23044225, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 3.9 g of sodium azide in 10 ml of water is added to a solution of 13.86 g (40 mmol) of p-toluenesulphonic acid (7-methoxy-1,2,3,4-tetrahydro-naphth-2-ylmethyl) ester in 200 ml of ethanol and the whole is boiled under reflux for 18 hours. After cooling, the alcohol is evaporated off under reduced pressure, water is added to the residue and extraction is carried out with dichloromethane. The organic phase is washed with water, dried over sodium sulphate and concentrated by evaporation. (7-methoxy-1,2,3,4-tetrahydro-naphth-2-yl)methylazide is obtained in the form of a yellow oil.

Aufarbeitung

  1. temperatureunder reflux for 18 hours
  2. temperatureAfter cooling
  3. customthe alcohol is evaporated off under reduced pressure, water
  4. additionis added to the residue and extraction
  5. washThe organic phase is washed with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-5d76f36805e24074808e522c6fd94208
Quelldatensatz
uspto-grants-1990_07
Patentnummer
US04939160

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