反应 #1135816
ord-8d0888b8740646e186ceb30047fdf103
反应方程式
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
收率 92.1%
反应物
试剂
无
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1萃取the mixtures were extracted with ethyl acetate
- 2洗涤the organic layers were washed with water and saturated saline
- 3干燥were dried over anhydrous magnesium sulfate
- 4浓缩were then concentrated under reduced pressure
实验过程
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.