反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
129 mg (1 mmol) of diisopropylethylamine was added to a suspension of 84 mg (0.42 mmol) of L-methionine methyl ester hydrochloride and 100 mg (0.35 mmol) of 2-[4-[(dimethylamino)methyl]phenyl]-3-oxa-1-azaspiro[4.5]dec-1-en-4-one in 3 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 saturated brine, followed by drying with 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 93 mg (59%) of the title compound.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux overnight
- distillationAfter the solvent was distilled off under reduced pressure, ethyl acetate
- additionwas added
- washthe mixture was washed with saturated brine
- dry with materialby drying with sodium sulfate
- distillationAfter the solvent was distilled off under reduced pressure, diethyl ether
- additionwas added
- filtrationThe precipitated solid was collected by filtration
- customdried under reduced pressure