利奈唑胺中间体的制备工艺优化

Optimization of the Preparation Process of Linezolid Intermediates

以3-氟-4-吗啉基硝基苯为原料,通过钯碳氢气还原合成得到3-氟-4-(4-吗啉基)苯胺,经重结晶提纯得到目标化合物,并对化合物进行了结构验证。结果表明,V(甲醇)∶V(水)=1∶4,溶剂用量(V/m)为5 m L/g时,精制效果最佳,总收率96.8%,脱氟杂质:4-(4-吗啉基)苯胺≤0.08%,产品纯度≥99.0%。本工艺反应条件温和,后处理操作简单,革除了以甲酸铵为氢源的钯碳反应体系中后处理操作繁琐的问题。

3-Fluorine-4-(4-morpholine)aniline was synthesized by Pd-C/H 2 reduction from 4-(3-fluoro-4-nitrophenyl)morpholine and the target compound was purified by recrystallization.The structure of the target compound was confirmed by 1H NMR.The optimal reaction conditions were as follows V(methanol)∶V(water)=1∶4,the solvent dosage(V/m)is 5 mL/g,the total yield is 96.8%,and defluorine impurity:4-(4-morpholine)aniline is less than 0.08%,and the product purity is greater than 99.0%.This process has the advantages of simple operation and mild condition,and is eliminating the complicated problems of post-processing operation in the Pd-C/HCOONH 4.