反应详情

A suspension of 4-[3-(benzhydryl-sulfamoyl)-propyl]-piperazine-1-carboxylic acid tert-butyl ester (650 mg, 1.37 mmol) and palladium hydroxide (1.154 g, 1.64 mmol, 20% w from Aldrich) in methanol (10 mL) was hydrogenated at room temperature overnight using a Parr apparatus (50 psi). The reaction mixture was filtered through a Celite cake, and the filtrate was concentrated. Purification of the crude residue by flash column chromatography (40 g of silica gel, eluting with methanol and ethyl acetate) gave 4-(3-sulfamoyl-propyl)-piperazine-1-carboxylic acid tert-butyl ester as an off-white solid (334 mg).

1. filtrationThe reaction mixture was filtered through a Celite cake
2. concentrationthe filtrate was concentrated
3. customPurification of the crude residue
4. washby flash column chromatography (40 g of silica gel, eluting with methanol and ethyl acetate)