Reaktion #1135816

Reaktionsgleichung

dimethyl sulfate

1-(2-methyl-3-ethoxyphenyl)-1,4-dihydrotetrazole-5-one

potassium carbonate

N,N-dimethylformamide

→

1-(2-methyl-3-ethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one

Ausbeute 92.1%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixtures were extracted with ethyl acetate
2. 2
   Waschenthe organic layers were washed with water and saturated saline
3. 3
   Trocknenwere dried over anhydrous magnesium sulfate
4. 4
   Einengenwere then concentrated under reduced pressure

Vorschrift

Under ice-cooling, to a mixture of 1-(2-methyl-3-ethoxyphenyl)-1,4-dihydrotetrazole-5-one 39.0 g, potassium carbonate 36.7 g and N,N-dimethylformamide 400 mL was added dimethyl sulfate 44.7 g and the resulting mixtures were raised to room temperature and were stirred for seven hours. Thereto was added water and the mixtures were extracted with ethyl acetate and the organic layers were washed with water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-(2-methyl-3-ethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 38.2 g.

Quelle