- Preparation method of non-natural amino acid N-fluorenylmethoxycarbonyl-beta-(2-thienyl)-D-alanine
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The invention discloses a preparation method of non-natural amino acid N-fluorenylmethoxycarbonyl-beta-(2-thienyl)-D-alanine, and mainly solves the technical problems that an original technology is complex in use, low in yield, high in cost, and the like. The preparation method comprises the steps of step I, carrying out chlorine acylation on 2-thiophene methanol through a chlorine acylating agent, so as to prepare 2-chloromethyl thiophene; step II, enabling 2-chloromethyl thiophene and diethyl acetamidomalonate to react through sodium ethoxide, so as to prepare 2-thienyl diethyl malonate; and step III, enabling 2-thienyl diethyl malonate subjected to alkaline saponification and L-acetyl transferase resolution to react with fmoc-groups, filtering an obtained L amino protection product, collecting a mother liquid, adding hydrochloric acid and a methyl alcohol solution for reflux reaction, monitoring the reaction process through NMR, adding fmoc-osu for reaction, tracking and monitoring the reaction process through TLC, and carrying out impurity extraction, acidification, and the like, to obtain the N-fluorenylmethoxycarbonyl-beta-(2-thienyl)-D-alanine.
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Paragraph 0016-0018; 0021-0023; 0026-0027; 0030-0031; 0038
(2017/05/13)
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