preparation | 25mmol of D-leucine is dissolved in 10ml of sodium hydroxide (NaOH) aqueous solution with a mass concentration of 10% at -5 ℃ to obtain the dissolved liquid. 35mmol (I .e. 4.5ml) of benzyl chloramate (Cbz-Cl) is added dropwise to the dissolved liquid at a rate of 1 drop/4 seconds while stirring for reaction, and drop the sodium hydroxide (NaOH) aqueous solution with a mass concentration of 10% to keep the PH at 8. After dropping, place it at 10°C, stir for 15 hours, use ninhydrin as the developer to develop color without purple, and then use 16ml/time Ether wash for 3 times, discard the ether, and get the aqueous phase. The aqueous phase is adjusted to 3 with concentrated hydrochloric acid with a mass concentration of 30%, and milky white solids appear, the liquid with milky white solid is extracted with 16ml/time of ethyl acetate for 3 times, merged, and the combined liquid is washed with 16ml/time of distilled water for 2 times, 16ml/time of saturated salt water for 1 time, and then dried with anhydrous magnesium sulfate for 10 hours, filtered, and the filtrate is concentrated under reduced pressure to obtain a light yellow oil. The mixed solvent prepared by ethyl acetate and petroleum ether with a volume ratio of 1:3 is used as the mobile phase, purification by chromatography column to obtain 4.0g CBZ-D-leucine, yield: 61.5%, anhydrous transparent oil. |