反应详情

To a stirred mixture of N-[(butylamino)carbonyl]-1-methyl-1H-benzotriazole-4-sulfonamide (8.25 g), 1,4-diazabicyclo[2,2,2]octane (catalytic amount), and xylenes (175 mL), heated at reflux under a nitrogen atmosphere, was added phosgene (2 mL) in small portions over 1 hour. The resulting suspension was heated an additional 0.5 hours and was cooled prior to filtering off the insoluble material. The filtrate was evaporated to give 3.05 g of the title compound as a pale yellow solid. IR (nujol) 2260 cm-1. The compound was immediately diluted to 100 mL with dry acetonitrile and stored under nitrogen to give a 0.125M solution of the title compound for further use.

1. temperatureheated
2. temperatureat reflux under a nitrogen atmosphere
3. temperatureThe resulting suspension was heated an additional 0.5 hours
4. temperaturewas cooled
5. filtrationto filtering off the insoluble material
6. customThe filtrate was evaporated