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

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.

1. stirringthe mixture was stirred at room temperature for 15 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionthe residue was diluted with an aqueous sodium bicarbonate solution
4. extractionextracted with dichloromethane
5. dry with materialThe extract was dried over anhydrous sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure

ORD record

ord-a3dbf606eac24f83aa90a21acc8dfd67

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08697865B2