目的 對(duì)（R）-（+）-脫水芽子堿甲酯的合成工藝進(jìn)行研究和結(jié)構(gòu)表征。方法 以托品酮為原料，經(jīng)克萊森縮合、拆分、還原和消除得到目標(biāo)產(chǎn)物，并以成鹽的方式得到其富馬酸鹽，以溶劑揮發(fā)法培養(yǎng)單晶，采用X射線單晶衍射對(duì)結(jié)晶形態(tài)進(jìn)行表征。結(jié)果 優(yōu)化了合成工藝，總收率為36%。測(cè)試結(jié)果表明不對(duì)稱單位化學(xué)計(jì)量式為C₁₄H₁₉NO₆，相對(duì)分子質(zhì)量為297.30，晶體密度為1.359 g/cm³，該晶胞屬于正交晶系，空間群為P2₁2₁2₁。結(jié)論 本合成工藝簡(jiǎn)化了實(shí)驗(yàn)操作，更適合大規(guī)模制備，且為脫水芽子堿的結(jié)構(gòu)確證提供了新的依據(jù)。

Objective To study the synthetic technology and accurate structure of (R)-(+)-Anhydroecgonine methyl ester. Methods Tropinone was used as starting materials to synthesize the target compound by a series of chemical reactions including Claisen condensation, resolution, reduction, and elimination. Evaporation method was used to grow single crystals of (R)-(+)-Anhydroecgonine methyl ester fumarate, which were then characterized using single crystal X-ray diffraction. Results The synthetic technology was optimized with the yield of 36%. Results showed that the unit stoichiometric of the single crystals was C₁₄H₁₉NO₆, and the relative molecular mass was 297.30, and crystal density was 1.359 g/cm³. The unit cell belonged to an orthorhombic system, and the space group was P2₁2₁2₁. Conclusion The synthetic technology simplifys the reaction procedure, and is more suitable for large-scaled preparation, which provides a new evidence for the structure confirmation of (R)-(+)-Anhydroecgonine methyl ester.

中國(guó)醫(yī)學(xué)科學(xué)院醫(yī)學(xué)與健康科技創(chuàng)新工程項(xiàng)目（2016-I2M-3-022、2017-I2M-3-019）