[Analysis of 1-(2,6-dichlorophenyl)-2-indolone and related materials by high performance liquid chromatography].
The separation of 1-(2,6-dichlorophenyl)-2-indolone (DCI) and related materials in the synthesis of medical intermediate DCI from 2, 6-dichlorophenol and phenylamine was investigated with high performance liquid chromatography under different chromatographic conditions. The results showed that DCI and related materials were in baseline separation by using CLC-CN(150 mm x 6.0 mm i.d., 7 microns) as column, MeOH-H2O(6:4, V/V) as mobile phase and a flow-rate at 1 mL/min. A rapid, accurate and reproducible HPLC method for determining DCI was developed. Fine and crude DCI samples were detected, results showed that N-(2,6-dichlorodiphenyl)-chloracetyl amide (CBCC) was the main impurity in fine sample, and CBCC and 2,6-dichlorodiphenylamine were the main impurities in the crude one.
Ji
Q M
QM
Laboratory of Biochemistry, Guangzhou Medical College, Guangzhou 510182, China. jqmlig@public.guangzhou.gd.cn
Zhang
S S
SS
Hao
Q X
QX
Liu
Y H
YH
Wu
Y J
YJ
D000814:Aniline Compounds / Q000302:isolation & purification*; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000138:chemical synthesis / Q000302:isolation & purification; D002733:Chlorophenols / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007211:Indoles / Q000302:isolation & purification
C476152:1-(2,6-dichlorophenyl)-2-indolone; D000814:Aniline Compounds; D000894:Anti-Inflammatory Agents, Non-Steroidal; D002733:Chlorophenols; D007211:Indoles; C032729:2,6-dichlorophenol