反应详情

温度

0 °C

To a solution of 0.50 g of (S)-(-)-2-azetidine carboxylic acid in 15 ml of 10 aqueous sodium carbonate solution was added 1.3 g of 9-fluorenylmethyl chloroformate in 10 ml of dioxane, dropwise, while maintaining the temperature of the reaction mixture at 0° C. The reaction mixture was allowed to warm to room temperature and stirred for 3 hours, then poured into water and the aqueous solution was washed with ether. The aqueous layer was cooled to 0° C. and adjusted to a pH of 2 with 3N hydrochloric acid and extracted with ethyl acetate. The ethyl acetate solution was dried over magnesium sulfate, filtered, and evaporated in vacuo to give (S)-N-(9-fluorenylmethoxycarbonyl) azetidine-2-carboxylic acid.

1. temperatureto warm to room temperature
2. washthe aqueous solution was washed with ether
3. temperatureThe aqueous layer was cooled to 0° C.
4. extractionextracted with ethyl acetate
5. dry with materialThe ethyl acetate solution was dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated in vacuo