反应详情

N-(2-Indanyl)glycine (1.0 g) is suspended in 10 ml of dimethylacetamide, then 2.0 g of 3-benzoylthio-2-methylpropionyl chloride is added dropwise with stirring at room temperature, and thereafter stirring is continued at room temperature for 2 hours. The reaction mixture is poured into 100 ml of water, and extracted with 200 ml of ethyl acetate. The extract is washed with 20 ml of 10% hydrochloric acid and with water, and dried over anhydrous sodium sulfate. After ethyl acetate is distilled off under reduced pressure, the residue is subjected to silica gel column chromatography and eluted with acetone-benzene (1:9). The oil obtained is crystallized from an ethyl ether-petroleum ether mixture, to give 1.4 g of N-(3-benzoylthio-2-methylpropionyl)-N-(2-indanyl)glycine, colorless needles showing a melting point of 113°-115° C.

1. stirringstirring
2. extractionextracted with 200 ml of ethyl acetate
3. washThe extract is washed with 20 ml of 10% hydrochloric acid and with water
4. dry with materialdried over anhydrous sodium sulfate
5. distillationAfter ethyl acetate is distilled off under reduced pressure
6. washeluted with acetone-benzene (1:9)
7. customThe oil obtained
8. customis crystallized from an ethyl ether-petroleum ether mixture