[Separation and purification of 2-chloro-5-trichloromethylpyridine from products of photochemical chlorination of 3-methylpyridine using preparative liquid chromatography].
A preparative high performance liquid chromatographic technique was used to separate and purify 2-chloro-5-trichloromethylpyridine from the products of photochemical chlorination with 3-methylpyridine as raw material. The elution mode, the flow rate of the mobile phase and injection volume were optimized. The optimum operation parameters were selected as follows: Zorbox-C,18 reversed-phase column with the flow rate gradient elution of 30% acetonitrile in water as the mobile phase (gradient elution program: 0 - 8 min at 4 mL/min, 8 - 14 min at 10 mL/min), and a diode array detector with wavelength set at 240 nm, injecting volume of 100 microL. The average recovery rate was 82.7% and relative standard deviation (RSD) was 4.0% (n = 5). High purity (99.01%) product was obtained. The effective and accurate method has been successfully applied to the preparation of pure 2-chloro-5-trichloromethylpyridine.
Su
Li
L
Southwest University of Science and Technology, Mianyang 621010, China. suli8825@126.com
Zhang
Yong
Y
Huang
Keming
K