反应详情

15.64 ml (80.0 mmol) of N-methyl-N-trimethylsilyltrifluoroacetamide was added to a suspension of 4.80 g (20.0 mmol) of 4-aminocatechol trifluoroacetate in 80 ml of dry acetonitrile. After stirring for 30 minutes, the dark solution was evaporated in vacuo and the dark residue was redissolved in 25 ml of dichloromethane. A solution of 4.56 g (20.0 mmol) of 2-(chlorocarbonyl)hydrazinecarboxylic acid, phenylmethyl ester in 50 ml of dichloromethane was slowly dropped in with stirring at 10° C. (40 minutes), and stirring was continued for 2 hours at room temperature. After evaporation in vacuo, the residue was taken up in a few ml of methanol and stirred until it became crystalline. The suspension was dluted with ether, and the precipitate was collected by suction; yield: 6.09 g, melting point 204° C., dec.

1. customthe dark solution was evaporated in vacuo
2. dissolutionthe dark residue was redissolved in 25 ml of dichloromethane
3. stirringwith stirring at 10° C. (40 minutes)
4. stirringstirring
5. waitwas continued for 2 hours at room temperature
6. customAfter evaporation in vacuo
7. stirringstirred until it
8. customthe precipitate was collected by suction