反応 #74277

反応方程式

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

methyl 2-(bromomethyl)benzoate

triethylamine

→

crude product

収率 51.0%

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

収率 51.0%

溶媒

benzene

反応条件

後処理

1. 1
   その他the resulting reaction mixture
2. 2
   温度was refluxed for 25 h
3. 3
   その他the solvent was evaporated under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
5. 5
   洗浄the organic layer was successively washed with water and brine
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 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%.

出典