反应详情

The mixture of 4-Chloro-2-nitro-benzenesulfonyl chloride (255 mg, 1 mmol), 4-Amino-piperidine-1-carboxylic acid tert-butyl ester (200 mg, 1 mmol) and K2CO3 (276 mg, 2 mmol) in DCM (3 mL) was stirred at room temperature for 1 hr. The mixture was concentrated in vacuo, the residue was dissolved in methanol, and then Ra—Ni (0.5 g) and hydrazine (1 mL, 17 mmol) was added. The resulting mixture was stirred at room temperature for 2 hr, filtered concentrated in vacuo. The residue was purified by column chromatography to give 380 mg 4-(2-Amino-4-chloro-benzenesulfonylamino)-piperidine-1-carboxylic acid tert-butyl ester as pale white solid. MS: [M+H]+=390

1. concentrationThe mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in methanol
3. stirringThe resulting mixture was stirred at room temperature for 2 hr
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography