反応 #61552

反応方程式

sodium thiosulfate

1H-Pyrazole-3,5-dicarboxylic acid diethyl ester

iodine

→

4-Iodo-1H-pyrazole-3,5-dicarboxylic acid diethyl ester

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度to reflux for 5 h
3. 3
   抽出The mixture was extracted with ethyl acetate (3×100 ml)
4. 4
   洗浄the combined organic layers were washed with water
5. 5
   乾燥dried over MgSO4
6. 6
   ろ過filtered
7. 7
   その他the solvents were removed under reduced pressure
8. 8
   ろ過The residue was filtered through a pad of silica gel eluting with heptane/ethyl acetate 1:1

実験手順

To a solution of 10 g 1H-Pyrazole-3,5-dicarboxylic acid diethyl ester in 400 ml acetonitrile 13 g ammonium cerium(iv) nitrate (CAN) and 7.17 g iodine were added and the mixture was heated to reflux for 5 h. Then, after cooling to RT, 30 ml sat. sodium thiosulfate solution were added. The mixture was extracted with ethyl acetate (3×100 ml), the combined organic layers were washed with water and then dried over MgSO4, filtered and the solvents were removed under reduced pressure. The residue was filtered through a pad of silica gel eluting with heptane/ethyl acetate 1:1.

出典