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 3-chloro-1-propanol 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 5 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 3-chloropropyl ester di(p-toluenesulfonate) in 88% yield; mp. 140°-145° C.

1. temperaturethe mixture was refluxed for 5 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