SU1002956A1 - Method of halogen-substituted phenylmethylbenzoilpyrazolon-5 chromatographic separation method - Google Patents

Description

(B) METHOD OF CHROMATOGRAPHIC SEPARATION OF HALOGEN SUBSTITUTED PHENYLMETHYLENZYLPYRAZOLONE-5

one

The invention relates to a new method for analyzing organic compounds, in particular, to the field of chromatographic analysis of organic compounds, halogen-substituted phenylmethylbenzoylpyrazolone-5 (FMBP-5).

These halogen-substituted FMBP-5 are widely used in analytical chemistry as complex-reagents, Q agents in extraction, biologically active substances in pharmacochemistry, herbicides and growth-regulating substances in agriculture, starting products for organic synthesis. ,five

A known method of separating FMBP-5 by electrochromatography on paper using a buffer solution with a pH containing 2.8 pyridine and 5 sorrel-2o acid as an electrolyte. The separations are conducted at a voltage of TsOO B and a current of 20 mA.

A known method of separating FMBP-5 on chromatographic plates of Silufol UV 25 in petroleum ether-diethyl ether-acetic acid 2 medium.

The aim of the invention is to provide a method for the separation of halogen-substituted PMBP-5, allowing for the separation of these compounds with sufficient accuracy.

The goal is achieved by the method of separation of halogen-substituted phenylmethylbenzoylpyrazolone-5, which consists in dissolving the analyte in chloroform by thin-layer chromatographic separation of it in a mixture of solvents: methyl ethyl ketone and hexane, taken in a volume ratio of 1: t-5, followed by treatment of the chromatogram obtained by UV light and followed by treatment of the obtained chromatograph with hexane and light and taken in a volume ratio of 1: t-5, followed by treatment of the chromatogram obtained by UV light and followed by treatment of the obtained chromatograph with hexane in a light and light: And-dimethylaminobenzaldehyde, or ferric chloride solution.

Example 1. On a fixed layer of silica gel LL-. At a distance of 1.5 cm from the edge of the plate, 0.01 ml of a solution of the analyzed sample in chloroform is applied. Chromatography is carried out using methyethyl ketone-hexane system (1 :,) for 20 minutes, with the solvent front moving 1 cm from the start line. In parallel with the test specimen Chromatograph the reference solutions on the same plate. After drying the chromatogram in air, the reagents are detected in UV-UV light (25 nm) in the form of dark layers on a fluorescent plate background. A layer of sorbent with a stain was transferred to a centrifuge tube, suspended in 3 ml of chloroform. After centrifuging, the liquid is photomized to a wavelength of 280 nm. Similarly, a blank experiment is carried out with an equal amount of free sorbent (with approximately the same Rjj value). Quantitative calculations are performed by comparing the eluate of the analyte with the eluate of a standard. P p i. measure 2. A fixed layer of silica gel at a distance of 1.5 cm from the edge of the plate is applied with 0.01 ml of a solution of the analyzed sample in chloroform. Chromatographic using an ascending method in the system methyl ethyl ketone-hexane (1: 4) for 20 min. Reference solutions are chromatographed on the same plate. After drying, the chromatogram is treated with 0, an alcoholic solution of i-dimethylaminobenzaldehyde. After heating to about 0.5 hours, the chromatograms containing the FMPP-5 derivatives turn yellow. The sorbents were transferred into centrifuge tubes, filled with 3 ml of ethanol, mixed and centrifuged. The colored liquid is photometrical at 480 nm and compared with the blank run. Example 3. On a fixed layer of silica gel, at a distance of 1.5 cm from the edge of the plate, 0.01 ml of a solution of the analyzed sample in chloroform was applied. Chromatographic using an ascending method in the system methyl ethyl ketone-hexane (1: 4) for 20 minutes. On the same plate chromatographic reference solutions. After drying, the chromatogram is treated with a FSC solution with a concentration of 1 mg / mol in 0.1 HCi. The chromatographic zones turn brown. The sorbents with patches are transferred to centrifuge tubes, pour 3 ml of ethanol, mix and centrifuge. The colored liquid is photometrized at 460 nm and compared with the blank run. The results of the analysis of the compounds by the proposed method are presented in Table. 1. Evaluation of the reproducibility of the results of the determination of halogen-substituted FMPP-5 in a simulating mixture is given in Table. 2. Table 1,

1-Phenyl-3 methyl-4- (4-chlorobenzoyl) -pyrazolone-5

1 -Phenyl-3-methyl-5 ("-chlorobenzoyl) -hydroxypyrazole-5

1-Phenyl-3 methyl-4, (4-chlorobenzoyl) -hydroxypyrazole-5

1-Phenyl-3-methyl-4- (4-bromobenzoyl) -pyrazolone-3

1-phenyl-3-methyl-5 (4-bromobenzoyl) -hydroxypyrazole-51-phenyl-3 methyl-C-chlorobenzoip) pisazolone-5

1-Phenyl 3 methyl-5

- {+ - hlarbenzoyl) hydroxypyrazole-5

1-phenyl-3 methyl-C, 5-Di (-chlorobenzoyl) -hydroxypyrazole-5

1-phenyl-3 methyl-4- (-bromobenzoyl) -pyrazolone-5

1-Phenyl-3 methyl-5 ("-bromobenzoyl) hydroxypyrazole-5

1-Phenyl-3 methyl, (-bromobenzoyl) -hydroxypyrazole-5

Continued table. one

table 2

IOtO.110 ± 0.15 10 ± 0.20

lOtO.OelOtO.I10i: 0.20

lOtO.IO iairO, 2 10iO, 25

lOirOJO 10i: 0.20 10iO, 20

10iO, 50 lOtO.IO 10 ± 0.35

10tO, 15 10tO, 15 1 (0.30

Compound

1-phenyl-3 methylpyra Formula of the invention. A method of chromatographic separation of halogen-substituted phenylmethylbenzoylpyrazolone-5, characterized in that the analyte solution is dissolved in chloroform and separated by thin-layer chromatography in a solvent mixture: methyl ethyl ketone and hexane taken in a volume ratio of 1: t-5) With the subsequent chromatography of the obtained chromatograph with ultraviolet light, either with a solution of VI-dimethylaminobenzaldehyde or with a solution of ferric chloride. Sources of information taken into account in the examination 1.Akimova TG, Terebenina AV, S Nava EM, Yordanov N., Borisov. G, Thin-layer chromatography and electrophoresis in the analysis of benzoyl 1-phenyl-Zmetil pyrazolone-5. ZAH 1980, 35, 8, p. 1561. 2. The same.

Claims (1)

Claim The method of chromatographic separation of halogen-substituted phenylmethylbenzoylpyrazolone-5, characterized in that the solution of the analyte is dissolved in chloroform and separated by thin layer chromatography in a mixture of solvents: methyl ethyl ketone and hexane taken in volume ^; in a winter ratio of 1: 4–5, followed by treatment of the obtained chromatogram with ultraviolet light, or a solution of Π-dimethylaminobenzaldehyde, or a solution of ferric chloride.