SU218173A1 - - Google Patents
Info
- Publication number
- SU218173A1 SU218173A1 SU1145102A SU1145102A SU218173A1 SU 218173 A1 SU218173 A1 SU 218173A1 SU 1145102 A SU1145102 A SU 1145102A SU 1145102 A SU1145102 A SU 1145102A SU 218173 A1 SU218173 A1 SU 218173A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dichlorophosphate
- mol
- chloroethyl
- ethyl
- chloro
- Prior art date
Links
- 238000001816 cooling Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- KITPBSLTXQKANT-UHFFFAOYSA-N chloro(2-hydroxyethoxy)phosphinous acid Chemical compound OCCOP(O)Cl KITPBSLTXQKANT-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000012442 inert solvent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ZMANZCXQSJIPKH-UHFFFAOYSA-N triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N 2-mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- KXOHONQCPYDQTC-UHFFFAOYSA-N chloro(dioxido)phosphane Chemical compound [O-]P([O-])Cl KXOHONQCPYDQTC-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Description
СПОСОБ ПОЛУЧЕНИЯ 5-|3-ХЛОРЭТИЛДИХЛОРФОСФАТА Изобретение касаетс спсоба получени неизвестного ранее соединени формулы ClaPSCHaCHaCl. II О S-p-Хлорэтилдихлорфосфат может найти применение в сельском хоз йстве. Предложено получать вещество взаимодействием монотиоэтиленгликольхлорфосфита хлором в инертном растворителе. Процесс ве дут ири охлаждении (желательно до ). Строение полученного соединени доказываетс химическими превращени ми. Л р и м е р. S-p-Хлорэгилдихлорфосфат. Газообразный хлор пропускают до проскока через раствор 6,9 г (0,0485 моль) монотиоэтиленгликольхлорфосфита в 20 мл сухого серного эфира при охлаждении реакционной смеси до . При перегонке получают 5,7 г (55,5i8/o) 3-(5-хлорэтилдихлорфосфата; т. 91-92 С (0,02 мм рт. ст.); df 1,552 1,5405; MRo пайдено 43,10; вычислено Пайдено, С1 48,54; 48,70; Р 14,23; S 15,83; 15,49. С2Н4С1зОР8. Вычислено, С1 49,87; Р 14,52; S 15,0. S-p-Хлорэтилдиэтилфосфат. С.месь 2,7 г (0,054 моль) этилового спирта и 5,5 г (0,054 моль) триэтиламина добавл ют по капл м при liO-15 С к раствору 5,5 г (0,027 моль) S-p-хлорэтилдихлорфосфата в 20 мл сухого серного эфира. При перегонке получают 2,3 г (37J/c) S-p-хлорэтилдиэтилфосфата, т. кип. 8S°C (0,01 мм рт. ст.); d4° 1,2260; ng 1,4825. Литературные данные; т. кип. (0,06 мм рт. ст.); df 1,2276; 1,4785, 1,4837. ИК-спектр (л,а,), CM-I: 1265 с. (Р-0), 565 ср. (Р-S), 1030 с. (Р-О-С). Предмет изобретени 1.Способ получени S-p-хлорэтилдихлорфосфата , отличающийс тем, что монотиоэтиленгликольхлорфосфит подвергают взаимодействию с хлором в инертном растворителе при охлаждении. 2.Способ по п. 1, отличающийс тем, что охлаждение ведут до .Method of production of 5- | 3-chloroethyl dichlorophosphate The invention relates to the preparation of a previously unknown compound of the formula ClaPSCHaCHaCl. II About S-p-Chloroethyl dichlorophosphate may be used in agriculture. It is proposed to obtain the substance by the interaction of monothioethylene glycol chlorophosphite with chlorine in an inert solvent. The process is carried out and cooled (preferably before). The structure of the obtained compound is proved by chemical transformations. LR and meer. S-p-Chloregyldichlorophosphate. Chlorine gas is passed through a solution of 6.9 g (0.0485 mol) of mono-ethylene glycol chlorophosphite in 20 ml of dry sulfuric ether while cooling the reaction mixture until. During distillation, 5.7 g (55.5i8 / o) of 3- (5-chloroethyl dichlorophosphate; t. 91-92 C (0.02 mm Hg); df 1.552 1.545; MRo; 43.10; calculated by Pajdeno, C1 48.54; 48.70; P 14.23; S 15.83; 15.49. C2H4C1ZOR8. Calculated, C1 49.87; R 14.52; S 15.0. Sp-Chloroethyl diethyl phosphate. A mixture of 2.7 g (0.054 mol) of ethyl alcohol and 5.5 g (0.054 mol) of triethylamine is added dropwise at liO-15 C to a solution of 5.5 g (0.027 mol) of Sp-chloro-ethyl dichlorophosphate in 20 ml of dry sulfuric acid. ether. During distillation, 2.3 g (37J / c) of Sp-chloro-ethyl diethylphosphate are obtained, bp 8S ° C (0.01 mmHg); d4 ° 1.2260; ng 1.4825. Literary data; kip. (0.06 mm Hg. Art.); df 1.2276; 1.4785, 1.4883. IR spectrum (l , a,), CM-I: 1265 p. (P-0), 565 cf. (P-S), 1030 p. (P-O-C). Subject of the invention 1. Method for producing Sp-chloro-ethyl dichlorophosphate, characterized by that mono ethylene glycol chlorophosphite is reacted with chlorine in an inert solvent during cooling. 2. The method of claim 1, wherein cooling is carried out before.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU218173A1 true SU218173A1 (en) |
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