反应详情

温度

-6 °C

14 ml. of N-ethyl piperidine was added to a solution of 23.3 grams of benzyloxycarbonyl alanine in 100 ml. of tetrahydrofuran and, after cooling to -10 degrees C., 14 ml. of sec. butyl chlorformate was added. Next, the mixture was stirred for 8 minutes and cooled to -6 degrees C. Then 30 ml. of a 4.1 solution of ethylamine in tetrahydrofuran was added. After 30 minutes of stirring at 0 degrees C. and 2 hours of stirring at room temperature, the reaction solution was evaporated, gradually shaken with a 5% solution of sodium hydrogen carbonate, with water, dried with anhydrous sodium carbonate, and evaporated. The evaporation residue was crystallized from ethyl acetate (30 ml.) and petroleum ether. 18.1 g of a product having a melting point of 116 to 117 degrees C. was obtained.

1. stirringAfter 30 minutes of stirring at 0 degrees C
2. stirringand 2 hours of stirring at room temperature
3. customthe reaction solution was evaporated
4. stirringgradually shaken with a 5% solution of sodium hydrogen carbonate, with water
5. dry with materialdried with anhydrous sodium carbonate
6. customevaporated
7. customThe evaporation residue was crystallized from ethyl acetate (30 ml.) and petroleum ether
8. customwas obtained