Reaktion #1135808

Reaktionsgleichung

methyl iodide

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

N,N-dimethylformamide

sodium hydride

→

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

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling
2. 2
   SonstigeTo the reaction mixtures
3. 3
   Temperaturcooling
4. 4
   TemperaturThe mixtures were raised to room temperature
5. 5
   workup.STIRRINGwere stirred for fourteen hours
6. 6
   SonstigeTo the reaction mixtures
7. 7
   Extraktionthe mixtures were extracted with ethyl acetate
8. 8
   WaschenThe organic layers were washed with 10% hydrochloric acid, water and saturated saline
9. 9
   Trocknenwere dried over anhydrous magnesium sulfate
10. 10
    Einengenwere then concentrated under reduced pressure

Vorschrift

To a mixture of the above-mentioned 1-(2-methyl-3-methoxyphenyl)-1,4-dihydrotetrazole-5-one 10.00 g and N,N-dimethylformamide 100 mL was added 55% sodium hydride 2.47 g under ice-cooling. The mixtures were raised to room temperature and were stirred for one hour. To the reaction mixtures was added methyl iodide 3.5 mL under ice-cooling. The mixtures were raised to room temperature and were stirred for fourteen hours. To the reaction mixtures was added water and the mixtures were extracted with ethyl acetate. The organic layers were washed with 10% hydrochloric acid, 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-methoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 2.19 g.

Quelle