GC/MS和NMR分析5-氟-2-硝基苯乙醚还原反应的副产物

Identification of by Products in the Reduction of 5-fluro-2-nitrophenetol by GC/MS and NMR

中文关键词:  4-氟-2-氯-6-乙氧基苯胺,5-氟-2-硝基苯乙醚,¹H-NMR,气质联用

英文关键词:4-fluor-2-chloro-6-ethoxyaniline,5-fluro-2-nitrophenetol,¹H-NMR,gas chromatography mass spectrometry

中文摘要:

      采用GC/MS分析5-氟-2-硝基苯乙醚的还原反应产物.在30.0 m×250 μm ZB-5MS毛细管柱上，载气为He气，流量为0.8 mL/min，起始柱温120 ℃维持3 min，以20 ℃/min的速率升至260 ℃并维持10 min，气化室温度270 ℃的条件下,5-氟-2-硝基苯乙醚还原的多种产物获得良好分离.通过对相应质谱图的解析,共鉴定出包括主产物在内的6种主要反应产物.经柱色谱分离提纯得到其中主要副产物，结合¹H-NMR确证该产物为未见报道过的副产物4-氟-2-氯-6-乙氧基苯胺.

英文摘要:

      The reduction products of 5-fluro-2-nitrophenetol were separated on a 30 m×0.25 mm ZB-5Ms capillary column. The helium gas flow rate was at 0.8 mL/min(consist flow), and oven temperature was held initially at 120 ℃ for three minutes, then elevated by 20 ℃/min to 260 ℃ and held for ten minutes. The injector temperature was 270 ℃. Few sample was introduced in GC by split injector .Five compounds were identified by GC/MS and the main by-product was validated by¹H-NMR as 4-fluor-2-chloro-6-ethoxyaniline, which had not been reported before.