SU341313A1 - Method of obtaining dichlorvinylalkyl (aryl) esters of 1-oxy-2,2,2-trichlorethylphosphinic acid - Google Patents

Description

The invention relates to the synthesis of new phosphororganic compounds - dichlorovinylalkyl (aryl) oxy esters of 1-OXY-2,2,2-trichloroethylphrsphinic acids - the general formula (OH) (, H-CC1 O) quality of biologically active substances The proposed method is new, since due to the elimination of NH | Ce phosphinate phosphonate rearrangement occurs and dichloro vinyl EPH5NL are formed, which are additionally esterified with alcohol. am.monium, subject to interaction with chloral in a molar ratio of 1: 2 when heated, preferably up to 80-100 ° C in an environment of a suitable organic solvent, for example, alcohol, followed by separation of the target product by known methods. (60 mmol) of dry ammonium hypophosphorite and 17.68 g (120 mmol) of chloral in 20 ml of ethyl alcohol are heated at 85 ° C with reflux condenser and stirrer for 1 h, then the temperature is raised to 95 ° C, incubated for 15 minutes. the mixture is cooled and filtered. The filtrate is evaporated in half, left for several hours and filtered. Both sediments are thoroughly washed with water and recrystallized from alcohol. The result is 6.3 g (30%) of the product. The table shows similarly obtained compounds and their constants.

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Claims (2)

The structure of the obtained products was determined on the basis of the data of elementary analysis, IR spectra, and NMR H spectra and double resonance. In the IR spectra of all compounds, there is no absorption in the region of 2300–2400 cm, which is characteristic of P – N bonds, while the spectra contain absorption bands at 3225–3240 (OH) and 1620–1630 cmH (). The NMR spectrum of the compound () was removed in dimethyl sulfoxide on an instrument RYa-2305 of SCR of the Academy of Sciences of the Academy of Sciences of the USSR (60 MHz). 3 С1зС-Сн (ONK dL. O-UHf-tH С1гС. СН-0 9 4.66 ppm - 4.8 Hz, .9-6 4.40 MD, - 6.8 Hz, 4.06 MD, H, 2 Hz in i S - 1.06 ppm Claim 1. A method for producing dichlorovinyl alkyl (aryl) 1-hydroxy-2,2, 2-Trichloroethylphosphinic acid esters, characterized in that the hypophosphorous acid salt, e.g. ammonium hypophosphite, is reacted with chloral in an organic solvent medium, e.g. alcohol, with heating and a molar ratio of 1: 2, followed by separation of the target product by known methods. 2. Method POP.1, characterized in that the process is conducted with ao-uo with.