Reaktion #305995

Reaktionsgleichung

2,6-Difluorobenzyl azide

propiolic acid

ascorbic acid

→

1-(2,6-Difluorobenzyl)-1H-1,2,3-triazole-4-carboxylic acid

Lösungsmittel

H2O tBuOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis kept at 25° C.
2. 2
   workup.WAITThe mixture is left
3. 3
   Sonstigethereby precipitating the product
4. 4
   FiltrationThe solid is filtered off on a Buchner
5. 5
   Filtrationfilter
6. 6
   Waschenwashed with ethyl ether
7. 7
   Sonstigedried under vacuum

Vorschrift

2,6-Difluorobenzyl azide (III) (7.0 g, 41.4 mmoles) is suspended in a H2O-tBuOH 1:1 mixture (120 ml), then propiolic acid (3.19 g, 45.6 mmoles), an ascorbic acid 1M solution (4.2 ml) and a CuSO4 0.3 M solution (1.4 ml) are added thereto. The reaction mixture is kept at 25° C. under stirring and is completed after 2 h. The mixture is left to cool at room temperature thereby precipitating the product. The solid is filtered off on a Buchner filter, washed with ethyl ether and dried under vacuum.

Quelle