反应详情

10 ml of N-methylmorpholine was added to 298 mg (2 mmol) of L-methionine and 259 mg (1 mmol) of 2-(4-methoxyphenyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one, and the mixture was stirred and heated under reflux overnight. The reaction solution was distilled off under reduced pressure, a 10% aqueous potassium hydrogensulfate solution was added thereto, and the mixture was extracted with methylene chloride three times. The obtained organic layer was dried with anhydrous sodium hydrogensulfate and the solvent was distilled off under reduced pressure. Ethyl acetate was added to the obtained residue, and the mixture was stirred overnight. The precipitated solid was collected by filtration and dried under reduced pressure to obtain 52 mg (13%) of the title compound.

1. temperatureheated
2. temperatureunder reflux overnight
3. distillationThe reaction solution was distilled off under reduced pressure
4. additiona 10% aqueous potassium hydrogensulfate solution was added
5. extractionthe mixture was extracted with methylene chloride three times
6. dry with materialThe obtained organic layer was dried with anhydrous sodium hydrogensulfate
7. distillationthe solvent was distilled off under reduced pressure
8. additionEthyl acetate was added to the obtained residue
9. stirringthe mixture was stirred overnight
10. filtrationThe precipitated solid was collected by filtration
11. customdried under reduced pressure