反应详情

温度

0 °C

10.6 ml of ethyl chlorocarbonate were gradually added, keeping the temperature below 0° C., to a solution of 15.8 g of 2-methyl-2-(2-thienyl)propionic acid [prepared as described in step (ii) above] and 15.6 ml of triethylamine in 210 ml of acetone. The reaction mixture was stirred at 0° C. for 2 hours, after which 110 ml of an aqueous solution containing 10.3 g of sodium azide were added to the mixture at 0° C. The reaction mixture was then stirred at 0° C. for 2 hours, diluted with water, and extracted three times with diethyl ether. The combined organic extracts were washed with 1N aqueous hydrochloric acid, with an aqueous solution of sodium hydrogencarbonate, and with a saturated solution of sodium chloride, in that order, after which it was dried over anhydrous magnesium sulfate, and concentrated by evaporation under reduced pressure to give 18.5 g of the title compound.

1. customthe temperature below 0° C.
2. additionwere added to the mixture at 0° C
3. stirringThe reaction mixture was then stirred at 0° C. for 2 hours
4. extractionextracted three times with diethyl ether
5. washThe combined organic extracts were washed with 1N aqueous hydrochloric acid, with an aqueous solution of sodium hydrogencarbonate
6. dry with materialwith a saturated solution of sodium chloride, in that order, after which it was dried over anhydrous magnesium sulfate
7. concentrationconcentrated by evaporation under reduced pressure