Piperazine → 1-[4-(Propan-2-yl)piperazin-1-yl]ethan-1-one

Temperature

60 °C

To a mixture of 12.95 g of piperazine, 0.75 g of sodium iodide and 3.46 g of potassium carbonate were added successively 25 ml of methanol and 6.15 g of 2-bromopropane and the mixture was stirred at 60° C. for 4 hours. Chloroform was added, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, 12 ml of acetic anhydride was added gradually and the mixture was stirred at room temperature for 2.5 hours. The reaction solution was poured into ice, chloroform was added and then it was neutralized with sodium carbonate. After extracted with chloroform, the extract was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue thus obtained was chromatographed over a silica gel column and the solvent was distilled off. The residue thus precipitated out was allowed to stand overnight and the diacetylpiperazine was filtered off to afford 7.26 g of the title compound as an oily substance.

1. washwashed with a saturated aqueous solution of sodium chloride
2. dry with materialdried over anhydrous magnesium sulfate
3. distillationThe solvent was distilled off under reduced pressure, 12 ml of acetic anhydride
4. additionwas added gradually
5. stirringthe mixture was stirred at room temperature for 2.5 hours
6. additionThe reaction solution was poured into ice, chloroform
7. additionwas added
8. extractionAfter extracted with chloroform
9. dry with materialthe extract was dried over anhydrous magnesium sulfate
10. distillationthe solvent was distilled off under reduced pressure
11. customThe residue thus obtained
12. customwas chromatographed over a silica gel column
13. distillationthe solvent was distilled off
14. customThe residue thus precipitated out
15. waitto stand overnight
16. filtrationthe diacetylpiperazine was filtered off

ORD record

ord-b5dd4437e0114128991029419f1f6eda

Source dataset

uspto-grants-1999_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05972943