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Gas chromatographic study of the chlorination of acetoacetic methyl ester

J. Hrivňák and Z. Veselá

Forschungsinstitut für agrochemische Technologie, Bratislava

 

Abstract: The chlorination of CH3COCH2CO2CH3 with Cl gas was described. For analysis of the reaction mixt., a rapid and simple gas chromatographic method was developed. The mixt. was analyzed in a glass column, 1.6-m. long and 4.6-mm. diam., filled with Celit 545 (granulation 0.16-20 mm.), contg. 13% bis(2-ethylhexyl) ester of sebacic acid and 2% poly(ethylene glycol) 400. The temp. of the column was 130° and the inflow of H was 95 ml./min. In the chlorination 2-chloro- and 2,2'-dichloroacetic acid methyl esters are formed. A chromatogram of the reaction mixt. contg. acetone, MeOH, EtOH, Me and Et acetoacetate, Me and Et 2-chloroacetoacetate and Me and Et 2,2'-dichloroacetoacetate is shown.

Full paper in Portable Document Format: 199a711.pdf (in Slovak)

 

Chemical Papers 19 (9) 711–714 (1965)

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