反应详情

温度

100 °C

A mixture of 1.0 gram of N2 -dansyl-L-arginine and 1.0 gram of p-toluenesulfonic acid monohydrate in 10 ml of n-butyl alcohol was heated for 30 minutes at 100° C. To the thus obtained clear solution, 100 ml of benzene was added, and the mixture was refluxed for 3 hours, removing water by azeotropic distillation. After the solvent was removed by distillation, 50 ml of ethyl ether and 50 ml of petroleum ether were added to the residue to give a crystalline mass. Crystallization from acetone gave N2 -dansyl-L-arginine-n-butyl ester di(p-toluenesulfonate) in 95% yield; mp. 160°-164° C.

1. temperaturethe mixture was refluxed for 3 hours
2. customremoving water
3. distillationby azeotropic distillation
4. customAfter the solvent was removed by distillation, 50 ml of ethyl ether and 50 ml of petroleum ether
5. additionwere added to the residue
6. customto give a crystalline mass
7. customCrystallization from acetone