反应详情

温度

50 °C

1.37 g (6.85 mmol) of 1,4-diazepane-1-carboxylic acid tert-butyl ester and 1.12 g (6.85 mmol) of benzoyl isothiocyanate were dissolved in 13 ml of THF and stirred at 50° C. for 2 h. The solvent was subsequently distilled off, and the residue was taken up in 34 ml of methanol and 3.4 ml of water, and 1.89 g of potassium carbonate were added. The mixture was boiled under reflux overnight and then filtered off. The filtrate was evaporated, slurried in 80 ml of water and extracted 3 times with 20 ml of EA each time. The organic phase was dried over sodium sulfate, filtered, evaporated, digested using a little PE and EA and filtered off with suction.

1. distillationThe solvent was subsequently distilled off
2. addition3.4 ml of water, and 1.89 g of potassium carbonate were added
3. temperatureunder reflux overnight
4. filtrationfiltered off
5. customThe filtrate was evaporated
6. extractionextracted 3 times with 20 ml of EA each time
7. dry with materialThe organic phase was dried over sodium sulfate
8. filtrationfiltered
9. customevaporated
10. filtrationfiltered off with suction