Methyl iodide → HCID 20483275, compound

To a solution of 6.4 g of 1-formyl-3-oxo-piperazine in 10 ml of anhydrous dimethylformamide was added 2.7 g of a sodium hydride (purity 53%) with ice-cooling, and the resulting mixture was reacted at room temperature for 1 hour. Subsequently, the mixture was incorporated with 7.1 g of methyl iodide and reacted for 10 hours. After the reaction, the dimethylformamide was removed by reduced pressure distillation to obtain 1-formyl-4-methyl-3-oxo-piperazine. This piperazine was dissolved in 70 ml of a 50% aqueous acetone solution containing 2.2 g of sodium hydroxide, and the resulting solution was reacted at room temperature for 3 hours. Thereafter, the solvent was removed by distillation under reduced pressure, and the residue was charged into acetone to deposit insolubles. The insolubles were separated by filtration, and the acetone was removed from the filtrate by distillation under reduced pressure. Subsequently, the residue was subjected to reduced pressure distillation to obtain 5.2 g of 1-methyl-2-oxo-piperazine, b.p. 104° C./4 mmHg, yield 91%.

1. temperaturecooling
2. customthe resulting mixture was reacted at room temperature for 1 hour
3. customreacted for 10 hours
4. customAfter the reaction
5. customthe dimethylformamide was removed by reduced pressure distillation

ORD record

ord-b01a5184538f4e32b7761d03b486aff3

Source dataset

uspto-grants-1980_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04219554