1-Piperazineacetic acid, 2-oxo-, 1,1-dimethylethyl ester

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of (2-oxo-piperazin-1-yl)acetic acid tert-butyl ester (1.22 g, 5.7 mmol) in 10 ml of methylene chloride is added triethylamine (1.2 mL, 8.55 mmol) and 6-chlorobenzothiophenesulfonyl chloride (1.52 g, 5.7 mmol). The reaction mixture is stirred overnight at ambient temperature. Flash column chromatography (50% ethyl acetate/hexane) affords 2.3 g (92%) of [4-(6-chlorobenzo[b]thiophene-2-sulfonyl)-2-oxopiperazine-1-yl]acetic acid tert-butyl ester.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 4-tert-Butoxycarbonylmethyl-3-oxopiperazine-1-carboxylic acid benzyl ester (2.0 g, 5.75 mmol) is dissolved in 20 mL of methanol and 2 mL of acetic acid. Palladium (5%) on carbon (100 mg) is added, and the reaction mixture is stirred in an atmosphere of hydrogen overnight. The mixture is filtered and concentrated. Ethyl acetate is added, and the mixture is neutralized to pH 7 using 1N NaOH. The organic layer is concentrated to give (2-oxo-piperazin-1-yl)acetic acid tert-butyl ester (1.22 g). The mixture is filtered concentrated Ethyl acetate is added The organic layer is concentrated