反应详情

温度

100 °C

A mixture of 1.0 gram of N2 -dansyl-L-arginine and 1.4 gram of p-toluenesulfonic acid monohydrate in 10 ml of 2-ethylhexanol was heated for 30 minutes at 100°C. To the thus otained clear solution, 100 ml of benzene was added, and the mixture was refluxed for 10 hours, removing water by azeotropic distillation. After the solvent was removed by distillation, 100 ml of ethyl ether was added to the residue to give a crystalline mass. Crystallization from acetone gave N2 -dansyl-L-arginine 2-ethylhexyl ester di(p-toluenesulfonate) in 91% yield; mp. 170°-174°C.

1. temperaturethe mixture was refluxed for 10 hours
2. customremoving water
3. distillationby azeotropic distillation
4. customAfter the solvent was removed by distillation, 100 ml of ethyl ether
5. additionwas added to the residue
6. customto give a crystalline mass
7. customCrystallization from acetone