反应详情

A total amount (260.3 g) of N-palmitoyloxy-succinimide synthesized above was suspended in 750 ml of DMF. To the suspension, a solution of Gly (56.3 g, 0.750 mol) and triethylamine (83.2 ml, 0.598 mol) in 250 ml of water was added dropwise with stirring while cooling with ice. The whole was stirred for 30 minutes while cooled with ice, then allowed to gradually reach room temperature, and stirred for 15 hours. An aqueous solution with pH 3 that was prepared by dissolving 100 ml of 6N hydrochloric acid in 1 L of water was stirred while cooled with ice. The reaction solution containing N-palmitoyloxy-succinimide was added dropwise to the aqueous solution. The precipitated solid was collected by filtration. The precipitated solid was washed with 2 L of water and then 1 L of hexane, and recovered to give 114 g (67%) of a target compound.

1. temperaturewhile cooling with ice
2. stirringThe whole was stirred for 30 minutes
3. temperaturewhile cooled with ice
4. customallowed to gradually reach room temperature
5. stirringstirred for 15 hours
6. customAn aqueous solution with pH 3 that was prepared
7. stirringwas stirred
8. temperaturewhile cooled with ice
9. additionwas added dropwise to the aqueous solution
10. filtrationThe precipitated solid was collected by filtration
11. washThe precipitated solid was washed with 2 L of water
12. custom1 L of hexane, and recovered