反应详情

A solution of 3-aminomethylpiperidine-1-carboxylic acid tert-butyl ester (2.20 g, 10.3 mmol) in dichloromethane (40 mL) was treated with triethylamine (1.90 mL, 13.3 mmol) and stirred on an ice bath. A solution of benzyl chloroformate (1.90 mL, 13.3 mmol) in dichloromethane (10 mL) was added over 5 minutes. The mixture was stirred at room temperature for 70 hours. It was washed with 0.1 N aqueous hydrochloric acid, dried over sodium sulfate, and concentrated under vacuum to provide a colorless gum (3.58 g, quantitative) which was used without further purification. 1H NMR (300 MHz, CDCl3) δ7.37 (m, 5H), 5.11 (s, 2H), 3.75 (m, 2H), 3.18 (m, 1H), 3.05 (m, 2H), 2.83 (m, 1H), 1.9-1.6 (m, 4H), 1.46 (s, 9H), 1.27 (m, 1H).

1. stirringThe mixture was stirred at room temperature for 70 hours
2. washIt was washed with 0.1 N aqueous hydrochloric acid
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under vacuum
5. customto provide a colorless gum (3.58 g, quantitative) which
6. customwas used without further purification