反应详情

To a mixture of piperidine-1,2-dicarboxylic acid 1-tert-butyl ester (5.32 g, 23.2 mmol) and triethylamine (4.04 g, 40 mmol) in THF (50 mL), isobutyl chloroformate (3.0 mL, 25.5 mmol) was added dropwise. After the mixture was stirred at room temperature for 45 min, 3-cyano-N-hydroxy-benzamidine (3.7 g, 23.2 mmol) and DMF (40 mL) were added. After being stirred for another hour, the reaction mixture was heated to 130˜135° C. for 1.5 h. Then the solution was cooled to room temperature and poured into water. Dichloromethane was used to extract the product. The organic layer was dried with sodium sulfate and concentrated in vacuo to give 8.1 g (98.4%) of the title compound as a thick brown oil.

1. additionwas added dropwise
2. stirringAfter being stirred for another hour
3. temperaturethe reaction mixture was heated to 130˜135° C. for 1.5 h
4. temperatureThen the solution was cooled to room temperature
5. extractionto extract the product
6. dry with materialThe organic layer was dried with sodium sulfate
7. concentrationconcentrated in vacuo