Trifluoroacetic acid → HCID 66645520, compound

1.0 ml of trifluoroacetic acid (13 mmol) was added to a solution of 0.40 g of 2,2-dimethyl-5-oxo-4-phenylpiperazine-1-carboxylic acid t-butyl ester obtained in the above reaction (1.31 mmol) in methylene chloride (2 ml) at room temperature, and the mixture was stirred at the same temperature for 30 minutes. The reaction mixture was concentrated under reduced pressure. A saturated sodium bicarbonate aqueous solution was added, followed by extraction with methylene chloride. Then, the organic layer was dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=10/1) to obtain 0.23 g of the title compound (yield: 99%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionA saturated sodium bicarbonate aqueous solution was added
3. extractionfollowed by extraction with methylene chloride
4. dry with materialThen, the organic layer was dried over anhydrous sodium sulfate
5. filtrationAfter filtration
6. customthe solvent was evaporated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=10/1)

ORD record

ord-4d10c451a2844e1fbdd691c543fba30a

Source dataset

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08158790B2