反応 #1135816

反応方程式

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

収率 92.1%

溶媒

water

反応条件

後処理

1. 1
   抽出the mixtures were extracted with ethyl acetate
2. 2
   洗浄the organic layers were washed with water and saturated saline
3. 3
   乾燥were dried over anhydrous magnesium sulfate
4. 4
   濃縮were then concentrated under reduced pressure

実験手順

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.

出典