反应详情

温度

-5 °C

To 100 ml of ethanol were added 9.69 g of N6-trifluoroacetyl-L-lysine and 8.16 g of trans-ethyl β-benzoylacrylate. Thereto was added 40 ml of 1N aqueous solution of lithium hydroxide over about 2 hours with stirring, while maintaining the temperature at about −5° C., and the stirring was further continued for 30 minutes. The reaction was terminated by adding 10 ml of concentrated hydrochloric acid thereto. To the reaction mixture were added 130 ml of ethanol and 5 g of 10% palladium-carbon, and a reduction reaction was carried out at about 40° C. under ordinary pressure. After the reaction, the catalyst was removed by suction filtration. The obtained ethanol solution was adjusted to about pH 4 with sodium hydroxide, added with water and concentrated under reduced pressure to distil away ethanol so as to replace the solvent with water. The resulting crystals were filtered with suction and dried under vacuum to give 33 g of N2-(1-ethoxycarbonyl-3-phenylpropyl)-N6-trifluoroacetyl-L-lysine (1S/1R ratio =80/20).

1. customThe reaction was terminated
2. additionby adding 10 ml of concentrated hydrochloric acid
3. additionTo the reaction mixture were added 130 ml of ethanol and 5 g of 10% palladium-carbon
4. customa reduction reaction
5. customwas carried out at about 40° C. under ordinary pressure
6. customAfter the reaction
7. customthe catalyst was removed by suction filtration
8. additionadded with water
9. concentrationconcentrated under reduced pressure
10. customto distil away ethanol so as
11. filtrationThe resulting crystals were filtered with suction
12. customdried under vacuum