反应详情

温度

10 °C

15.3 g of sodium hydride (65% dispersion in mineral oil, 0.414 moles) was suspended in 250 ml of N,N-dimethylformamide at 10° C. To this suspension, 100 g of 4-benzyl-2-oxo-3-phenylpiperazine (0.376 moles) was added portionwise over a period of 30 min and stirred for 15 min. A solution of 64 g of methyl iodide (0.45 moles) in 50 ml of N,N-dimethylformamide was added slowly in 45 min maintaining the temperature below 25° C. and maintained for 1 hour. After completion of the reaction, mass was poured slowly in 1000 ml of cold water (15° C.). The product was extracted with toluene (1×500 ml, 1×300 ml) from aqueous phase. Toluene layer was washed with water (2×200 ml) and concentrated. To the residue, 250 ml of cyclohexane was added and cooled to 10° C. with stirring. Filtered the product and washed with precooled cyclohexane to obtain 98.5 g of 4-benzyl-1-methyl-2-oxo-3-phenylpiperazine product (yield: 93.8%, purity: 99.15 by HPLC)

1. temperaturemaintaining the temperature below 25° C.
2. temperaturemaintained for 1 hour
3. customAfter completion of the reaction, mass
4. extractionThe product was extracted with toluene (1×500 ml, 1×300 ml) from aqueous phase
5. washToluene layer was washed with water (2×200 ml)
6. concentrationconcentrated
7. additionTo the residue, 250 ml of cyclohexane was added
8. stirringwith stirring
9. filtrationFiltered the product
10. washwashed with precooled cyclohexane