反应详情

温度

0 °C

0.84 g of 1,1-dimethyl-2-propynol and solution F were mixed and stirred for 15 minutes at 0° C. To the mixture was added 0.97 ml of 2-chloropropionyl chloride and the solution was stirred for 5 minutes at 0° C., additional 5 hours at room temperature. Then, to the reaction mixture was added 1N hydrochloric acid and water, and extracted with ethyl acetate. The organic layer was washed successively with water and aqueous solution of sodium bicarbonate, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was subjected to silica gel column chromatography to give 1.06 g of (1,1-dimethyl-2-propynyl) 2-chloropropionate.

1. stirringthe solution was stirred for 5 minutes at 0° C., additional 5 hours at room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed successively with water and aqueous solution of sodium bicarbonate
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue obtained