反応 #48510

反応方程式

Lithium bis(trimethylsilyl)amide

1-(4-benzylpiperazin-1-yl)tetrahydropyrimidin-2(1H)-one

Methyl iodide

→

title compound

1-(4-Benzylpiperazin-1-yl)-3-methyltetrahydropyrimidin-2(1H)-one

溶媒

THF

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 15 hours
2. 2
   濃縮The reaction mixture was concentrated under reduced pressure
3. 3
   workup.ADDITIONthe residue was diluted with an aqueous sodium bicarbonate solution
4. 4
   抽出extracted with dichloromethane
5. 5
   乾燥The extract was dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

実験手順

Lithium bis(trimethylsilyl)amide (1M THF solution; 1.5 mL) was added to a solution of 1-(4-benzylpiperazin-1-yl)tetrahydropyrimidin-2(1H)-one (0.27 g) obtained in Example 25a) in THF (10 mL) at 0° C., and the mixture was stirred at room temperature for one hour. Methyl iodide (0.09 mL) was added thereto, and the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with an aqueous sodium bicarbonate solution, and extracted with dichloromethane. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain the title compound (0.30 g, quantitative) as a brown oil.

出典