反应详情

温度

0 °C

0.60 g of methyl N-[2-chloro-5-(3-hydroxy-3-methyl-1-butynyl)benzyl]carbamate was dissolved in 10 ml of toluene. This solution was added at 0° C. to a mixture comprising 0.12 g of calcium chloride, 0.08 g of copper(I) iodide, 0.01 g of copper and 10 ml of concentrated hydrochloric acid, followed by stirring at 0° C. for 5 hours. This solution was poured into water and extracted with ethyl acetate, followed by drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude product was dissolved in 10 ml, of methanol. To this solution, 0.50 g of sodium methylate (28 wt % methanol solution) was added at room temperature, followed by stirring at room temperature for 24 hours. The reaction mixture was poured into water and extracted with ethyl acetate, followed by drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified with silica gel column chromatography to obtain 0.52 g of methyl N-[2-chloro-5-(3-methoxy-3-methyl-1-butynyl)benzyl]carbamate as a brown viscous liquid.

1. extractionextracted with ethyl acetate
2. dry with materialby drying over anhydrous magnesium sulfate
3. distillationThe solvent was distilled off under reduced pressure
4. customthe obtained crude product
5. stirringby stirring at room temperature for 24 hours
6. extractionextracted with ethyl acetate
7. dry with materialby drying over anhydrous magnesium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customthe residue was purified with silica gel column chromatography