Ethyl bromoacetate → HCID 16290587, compound

In N,N-dimethylformamide (50 ml) was dissolved 1-(tert-butoxycarbonyl)piperazine (942 mg). After the addition of triethylamine (1.40 ml), ethyl bromoacetate (1.13 ml) was added, followed by stirring overnight at room temperature. The reaction mixture was concentrated under reduced pressure. Ethyl acetate was added to the residue and the mixture was washed with water. The organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by chromatography on a silica gel column (hexane:ethyl acetate=3:1), whereby a colorless foam was obtained. The resulting substance was dissolved in a saturated hydrochloric acid—ethanol solution (10 ml) and the resulting solution was concentrated under reduced pressure. The solid thus precipitated was collected by filtration while being washed with ethyl acetate, whereby the title compound (841 mg) was obtained as a colorless solid.

1. additionwas added
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionEthyl acetate was added to the residue
4. washthe mixture was washed with water
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customThe residue was purified by chromatography on a silica gel column (hexane:ethyl acetate=3:1), whereby a colorless foam
8. customwas obtained
9. concentrationthe resulting solution was concentrated under reduced pressure
10. customThe solid thus precipitated
11. filtrationwas collected by filtration
12. washwhile being washed with ethyl acetate, whereby the title compound (841 mg)
13. customwas obtained as a colorless solid

ORD record

ord-b0774d3d4e614efb93ab18f91180eb93

Source dataset

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06747023B1