반응 #74277

반응 방정식

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

methyl 2-(bromomethyl)benzoate

triethylamine

→

crude product

수율 51.0%

2-((1-Benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidin-4-yl)methyl)-isoindolin-1-one

수율 51.0%

용매

benzene

반응 조건

후처리

1. 1
   기타the resulting reaction mixture
2. 2
   온도was refluxed for 25 h
3. 3
   기타the solvent was evaporated under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
5. 5
   세척the organic layer was successively washed with water and brine
6. 6
   건조The organic layer was dried over sodium sulfate
7. 7
   기타the solvent was evaporated under reduced pressure

실험 절차

To a solution of (1-benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidin-4-yl)methanamine (see above: synthesis of amine AM12) (1.22 mmol, 1.0 equiv.) and methyl 2-(bromomethyl)benzoate (1.22 mmol, 1.0 equiv.) in benzene (3 ml/mmol) was added triethylamine (2.44 mmol, 2.0 equiv.) and the resulting reaction mixture was refluxed for 25 h. The mixture was cooled to room temperature and the solvent was evaporated under reduced pressure. The residue was dissolved in ethyl acetate and the organic layer was successively washed with water and brine. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure to give the crude product which was purified by silica gel column chromatography. Yield: 51%.

출처