反应详情

679 mg (5.3 mmol) of diisopropylethylamine was added to a suspension of 419 mg (2 mmol) of L-methionine methyl ester hydrochloride and 500 mg (1.75 mmol) of 2-(2-benzothienyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one in 10 ml of toluene, and the mixture was heated under reflux overnight. After the solvent was distilled off under reduced pressure, ethyl acetate was added thereto, and the mixture was washed with a 10% aqueous potassium hydrogensulfate solution and saturated brine, followed by drying with anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, diethyl ether was added thereto, and the mixture was stirred overnight. The precipitated solid was collected by filtration and dried under reduced pressure to obtain 678 mg (86%) of the title compound.

1. temperaturethe mixture was heated
2. temperatureunder reflux overnight
3. distillationAfter the solvent was distilled off under reduced pressure, ethyl acetate
4. additionwas added
5. washthe mixture was washed with a 10% aqueous potassium hydrogensulfate solution and saturated brine
6. dry with materialby drying with anhydrous sodium sulfate
7. distillationAfter the solvent was distilled off under reduced pressure, diethyl ether
8. additionwas added
9. filtrationThe precipitated solid was collected by filtration
10. customdried under reduced pressure