반응 #1135816

반응 방정식

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

수율 92.1%

용매

water

반응 조건

후처리

1. 1
   추출the mixtures were extracted with ethyl acetate
2. 2
   세척the organic layers were washed with water and saturated saline
3. 3
   건조were dried over anhydrous magnesium sulfate
4. 4
   농축were then concentrated under reduced pressure

실험 절차

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.

출처