反应详情

Methanesulfonyl chloride (0.7 mL, 9.0 mmol) was added to a cooled solution of 4-(2-amino-ethyl)-piperazine-1-carboxylic acid tert-butyl ester (1.33 g, 5.8 mmol) in pyridine (25.0 mL). The reaction was stirred for 12 h and partitioned between partitioned between aqueous sodium bicarbonate and methylene chloride. The organic phase was washed with 1 M hydrochloric acid, aqueous sodium bicarbonate, and brine, dried over anhydrous magnesium sulfate and concentrated. Purification of the crude residue by chromatography over silica gel using 0-5% methanol in methylene chloride gave 4-(2-methanesulfonylamino-ethyl)-piperazine-1-carboxylic acid tert-butyl ester (0.70 g, 70%).

1. custompartitioned
2. custombetween partitioned between aqueous sodium bicarbonate and methylene chloride
3. washThe organic phase was washed with 1 M hydrochloric acid, aqueous sodium bicarbonate, and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customPurification of the crude residue by chromatography over silica gel using 0-5% methanol in methylene chloride