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×250μm 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.
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.
出处
《分析测试技术与仪器》
CAS
2008年第1期38-41,共4页
Analysis and Testing Technology and Instruments
