반응 #74273

반응 방정식

LAH

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

H2SO4

→

desired product

수율 90.0%

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

수율 90.0%

용매

THF

THF

THF

반응 조건

후처리

1. 1
   온도To a cooled
2. 2
   온도was heated to 50° C. for 12 h
3. 3
   기타The mixture was quenched with sodium sulfate solution
4. 4
   여과filtered through celite
5. 5
   세척washed with ethyl acetate
6. 6
   건조The organic layer was dried over sodium sulfate
7. 7
   기타the solvent was evaporated under reduced pressure

실험 절차

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%

출처