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

Temperature

60 °C

To 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. After the addition of chloroform and washing with a saturated aqueous solution of sodium chloride, the mixture was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, 12 ml of acetic anhydride was slowly added and the mixture was stirred at room temperature for 2.5 hours. The reaction solution was poured into ice and chloroform was added and the mixture was neutralized with sodium carbonate. After extracting with chloroform, the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the residue thus obtained was chromatographed over a silica gel column. The solvent was distilled off and the residue was allowed to stand overnight. The diacetylpiperazine thus precipitated out was filtered off to afford 7.26 g of the title compound as an oily substance.

1. washwashing with a saturated aqueous solution of sodium chloride
2. dry with materialthe mixture was dried over anhydrous magnesium sulfate
3. distillationThe solvent was distilled off under reduced pressure, 12 ml of acetic anhydride
4. additionwas slowly added
5. stirringthe mixture was stirred at room temperature for 2.5 hours
6. additionThe reaction solution was poured into ice and chloroform
7. additionwas added
8. extractionAfter extracting 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. waitto stand overnight
15. customThe diacetylpiperazine thus precipitated out
16. filtrationwas filtered off

ORD record

ord-ab004de9e77242eeaf0b66d58115bfd2

Source dataset

uspto-grants-2000_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06046201