Reaktion #305996

Reaktionsgleichung

2,6-Difluorobenzyl azide

methyl propiolate

Methyl propiolate

ascorbic acid

→

Methyl 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylate

Ausbeute 94.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis kept at 25° C.
2. 2
   EinengenThe mixture is concentrated
3. 3
   Waschenwashed with an ammonia diluted solution
4. 4
   SonstigeThe organic phase is dried
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated under reduced pressure
7. 7
   SonstigeA crystalline white solid is obtained in 94% yield

Vorschrift

2,6-Difluorobenzyl azide (3.0 g, 17.7 mmoles) is suspended in ethanol (30 ml), then methyl propiolate (IV) (1.6 g, 19.6 mmoles), ascorbic acid (317 mg, 1.8 mmoles) and CuSO4 pentahydrate (50 mg, 0.18 mmole) are added. The reaction mixture is kept at 25° C. under stirring overnight. The mixture is concentrated, taken up with ethyl acetate and washed with an ammonia diluted solution. The organic phase is dried, filtered, concentrated under reduced pressure. A crystalline white solid is obtained in 94% yield.

Quelle