反応 #74273

反応方程式

LAH

1-benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidine-4-carbonitrile

H2SO4

→

desired product

収率 90.0%

(1-Benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidin-4-yl)methanamine

収率 90.0%

溶媒

THF

THF

THF

反応条件

後処理

1. 1
   温度To a cooled
2. 2
   温度was heated to 50° C. for 12 h
3. 3
   その他The mixture was quenched with sodium sulfate solution
4. 4
   ろ過filtered through celite
5. 5
   洗浄washed with ethyl acetate
6. 6
   乾燥The organic layer was dried over sodium sulfate
7. 7
   その他the solvent was evaporated under reduced pressure

実験手順

To a cooled (0° C.) suspension of LAH (9.24 mmol, 3.0 equiv.) in THF (2 ml/mmol) was added dropwise conc. H2SO4 (4.62 mmol, 1.5 equiv.) in THF (1 ml/mmol) and the resulting suspension was stirred at room temperature for 1.5 h. A solution of 1-benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidine-4-carbonitrile (3.08 mmol, 1.0 equiv.) in THF (2 ml/mmol) was added dropwise to the reaction mixture and it was heated to 50° C. for 12 h. The mixture was quenched with sodium sulfate solution, filtered through celite and washed with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure to yield the desired product. Yield: 90%

出典