반응 #161062

반응 방정식

hydrochloric acid

2-[(E)-2-(2-furanyl)ethenyl]-3-oxo-1-azaspiro[4.5]dec-1-en-4-one

L-methionine

ethyl acetate

→

title compound

수율 9.0%

N-[[1-[[(E)-3-(2-Furanyl)-1-oxo-2-propenyl]amino]cyclohexyl]carbonyl]-L-methionine

수율 9.0%

용매

N-methylmorpholine

water

반응 조건

후처리

1. 1
   온도under reflux for 15 hours
2. 2
   기타The organic layer was separated
3. 3
   세척successively washed with water and saturated brine
4. 4
   건조by drying with anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONAfter the solvent was distilled off under reduced pressure
6. 6
   기타the residue was purified by silica gel chromatography

실험 절차

A solution of 491 mg (2 mmol) of 2-[(E)-2-(2-furanyl)ethenyl]-3-oxo-1-azaspiro[4.5]dec-1-en-4-one and 597 mg (4 mmol) of L-methionine in 20 ml of N-methylmorpholine was heated under reflux for 15 hours. After ethyl acetate and water were added to the reaction solution, the mixture was acidified using concentrated hydrochloric acid. The organic layer was separated and successively washed with water and saturated brine, followed by drying with anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the residue was purified by silica gel chromatography to obtain 74 mg (9%) of the title compound.

출처