Реакция #74273

Уравнение реакции

LAH

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

H2SO4

→

desired product

Выход 90.0%

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

Выход 90.0%

Растворители

THF

THF

THF

Условия реакции

Обработка

1. 1
   ТемператураTo a cooled
2. 2
   Температураwas heated to 50° C. for 12 h
3. 3
   ДругоеThe mixture was quenched with sodium sulfate solution
4. 4
   Фильтрацияfiltered through celite
5. 5
   Промывкаwashed with ethyl acetate
6. 6
   СушкаThe organic layer was dried over sodium sulfate
7. 7
   Другоеthe solvent was evaporated under reduced pressure

Методика

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%

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