反応 #1135793

反応方程式

methyl iodide

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

N,N-dimethylformamide

sodium hydride

→

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

溶媒

water

反応条件

後処理

1. 1
   温度cooling
2. 2
   その他To the reaction mixtures
3. 3
   温度cooling
4. 4
   温度The mixtures were raised to room temperature
5. 5
   workup.STIRRINGwere stirred for fourteen hours
6. 6
   その他To the reaction mixtures
7. 7
   抽出the mixtures were extracted with ethyl acetate
8. 8
   洗浄The organic layers were washed with 10% hydrochloric acid, water and saturated saline
9. 9
   乾燥were dried over anhydrous magnesium sulfate
10. 10
    濃縮were then concentrated under reduced pressure

実験手順

To a mixture of the above-mentioned 1-(2-methyl-3-fluorophenyl)-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-fluorophenyl)-4-methyl-1,4-dihydrotetrazole-5-one 2.19 g.

出典