反応 #1062

反応方程式

compound ( 4 )

4-(4-phenoxyphenyl)piperidine

chloroacetonitrile

sodium iodide

potassium carbonate

→

compound ( 26 )

収率 91.0%

1-cyanomethyl-4-(4-phenoxyphenyl)piperidine

収率 91.0%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   温度This was then heated
2. 2
   温度at reflux for 2 hours
3. 3
   抽出extraction
4. 4
   その他The extract was dried
5. 5
   ろ過filtered
6. 6
   濃縮concentrated under reduced pressure
7. 7
   その他to obtain a residue which
8. 8
   その他was then purified by silica gel column chromatography (methylene chloride:methanol =30:1)

実験手順

To an 8 ml dimethylformamide solution of 300 mg of the compound (4) synthesized in Reference Example 4 were added 93 mg of chloroacetonitrile, 355 mg of sodium iodide, and 196 mg of potassium carbonate. This was then heated at reflux for 2 hours. To the reaction was added 10 ml of ice water, then extraction was performed with ethyl acetate. The extract was dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol =30:1) to obtain the above-identified compound (26) in an amount of 313 mg (yield of 91%).

出典