反应详情

To an ice-cooled suspension of 1.0 gram of N2 -dansyl-L-arginine in 15 ml of methanol was added dropwise 0.5 ml of thionyl chloride with vigorous stirring. After being allowed to stand for 2 hours at room temperature, the reaction mixture was refluxed for 2 hours, and was evaporated to dryness (syrup). Treatment of the residual syrup with cold ethyl ether and a small amount of water gave crude crystals. After recrystallization from methanol-ethyl ether, colorless N2 -dansyl-L-arginine methyl ester dihydrochloride monohydrate was obtained in 92% yield: mp. 147°-150° C.

1. temperaturethe reaction mixture was refluxed for 2 hours
2. customwas evaporated to dryness (syrup)
3. customTreatment of the residual syrup with cold ethyl ether and a small amount of water gave crude crystals
4. customAfter recrystallization from methanol-ethyl ether