171778-17-9Relevant articles and documents
Synthesis method of Na-9-fluorenylmethoxycarbonyl-O-acetyl-L-serine
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Paragraph 0014; 0028; 0029; 0030, (2018/04/01)
The invention relates to a synthesis method of Na-9-fluorenylmethoxycarbonyl-O-acetyl-L-serine, mainly aiming at solving the technical problems that in the existing synthesis method, the aftertreatment operation is more troublesome since perchloric acid is taken as a catalyst, excessive acetyl chloride is used, and potential safety hazard is caused when ethyl ether is used for crystallizing. The method comprises the following steps: (1) dissolving solid L-serine into an acetic acid solution, dropwise adding liquid acetyl chloride, and stirring for carrying out reaction; adding the reaction liquid into a petroleum ether solution, separating out an intermediate O-acetyl-L-serine, filtering and drying; (2) dissolving the intermediate into a sodium carbonate solution, dropwise adding a 9-fluorene methyl-N-succinimido-carbonate solution dissolved in ethyl acetate, removing the excessive 9-fluorene methyl-N-succinimido-carbonate in a layering way, acidifying the water phase by using hydrochloric acid, then extracting by using an extracting agent-ethyl acetate, washing the obtained oil phase with water, removing the hydrochloric acid, and concentrating the oil phase for removing the extracting agent-ethyl acetate so as to obtain the white crystal Na-9-fluorenylmethoxycarbonyl-O-acetyl-L-serine product. The product synthesized by the method is an important raw material for synthesizing polypeptide drugs.