反应详情

30 mg of 10% palladium-carbon was added to a solution of 350 mg (1 mmol) of N—[N-[(phenylmethoxy)carbonyl]-L-leucyl]-L-valinol obtained in Reference example 178 in 10 ml of methanol, and the mixture was stirred under a hydrogen atmosphere at room temperature overnight. After the reaction solution was filtered, the filtrate was concentrated under reduced pressure. 10 ml of ethyl acetate, 10 ml of water and further 159 mg (1.5 mmol) of sodium carbonate were added to the residue. A solution of 131 mg (1 mmol) of 2-furancarbonyl chloride in 3 ml of ethyl acetate was added to the mixture solution under ice-cooling. The reaction solution was returned to room temperature and stirred overnight. The aqueous layer of reaction solution was separately collected and extracted with ethyl acetate. The organic layer was combined and after it was washed with 10% potassium hydrogensulfate, and then saturated brine, it was dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, ether was added to the residue, and the crystal was washed to obtain 268 mg (86%) of the title compound.

1. filtrationAfter the reaction solution was filtered
2. concentrationthe filtrate was concentrated under reduced pressure
3. temperaturecooling
4. customwas returned to room temperature
5. stirringstirred overnight
6. customThe aqueous layer of reaction solution
7. customwas separately collected
8. extractionextracted with ethyl acetate
9. washafter it was washed with 10% potassium hydrogensulfate
10. dry with materialsaturated brine, it was dried with anhydrous sodium sulfate
11. distillationThe solvent was distilled off under reduced pressure, ether
12. additionwas added to the residue
13. washthe crystal was washed