SU172326A1 - METHOD OF OBTAINING 0, O-DIMETHYL-2,2,2-TRICHLOR-1-OXYETHYLPHOSPHONATE (CHLOROPHOSE) - Google Patents
METHOD OF OBTAINING 0, O-DIMETHYL-2,2,2-TRICHLOR-1-OXYETHYLPHOSPHONATE (CHLOROPHOSE)Info
- Publication number
- SU172326A1 SU172326A1 SU885907A SU885907A SU172326A1 SU 172326 A1 SU172326 A1 SU 172326A1 SU 885907 A SU885907 A SU 885907A SU 885907 A SU885907 A SU 885907A SU 172326 A1 SU172326 A1 SU 172326A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dimethyl
- oxyethylphosphonate
- chlorophose
- trichlor
- obtaining
- Prior art date
Links
- 229960001952 metrifonate Drugs 0.000 description 6
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 description 6
- HFFLGKNGCAIQMO-UHFFFAOYSA-N Chloral Chemical compound ClC(Cl)(Cl)C=O HFFLGKNGCAIQMO-UHFFFAOYSA-N 0.000 description 5
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- SMZHKGXSEAGRTI-UHFFFAOYSA-N 1,1,1-trichloropropan-2-one Chemical compound CC(=O)C(Cl)(Cl)Cl SMZHKGXSEAGRTI-UHFFFAOYSA-N 0.000 description 1
- 235000019755 Starter Diet Nutrition 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 150000002373 hemiacetals Chemical class 0.000 description 1
- 239000007788 liquid Substances 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
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940029273 trichloroacetaldehyde Drugs 0.000 description 1
Description
Изгзестеи способ получени 0,0-диметил2 ,2,2-трихлор-1-оксиэтилфосфоната (хлорофоса ) взаимодействием диметилфосфита с трихлорацетальдегидом (хлоралем).Igstesy is a method for producing 0,0-dimethyl2, 2,2-trichloro-1-hydroxyethylphosphonate (chlorophos) by reacting dimethylphosphite with trichloroacetaldehyde (chloral).
При получении хлорал из этилового спирта последн стади св зана с обработке) хлормасла серной кислотой.In the preparation of chloral from ethyl alcohol, the latter is associated with the treatment of chlorine oil with sulfuric acid.
Предлагаемый способ получени хлорофоса более простой. Вместо хлорал используетс промежуточный продукт - полуацеталь хлорал . При этом стади выделени хлорал исключаетс .The proposed method for producing chlorophos is simpler. Instead of chloral, an intermediate is used - chloral hemiacetal. At this stage, the release of chloral is excluded.
Пример. В трехгорлую колбу, снабженную мешалкой, термометром и обратным холодильником , помещают 97 г (0,5 моль) моноэтилальхлорал и 55 г (0,5 моль) диметилфосфита . При 75-80°С смесь, перемешива , выдерживают 3-4 час.Example. In a three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, 97 g (0.5 mol) of monoethyl alloral and 55 g (0.5 mol) of dimethyl phosphite are placed. At 75-80 ° C, the mixture is stirred for 3-4 hours.
После этого под вакуумом (30 мм рт. ст.) и температуре куба 90°С отпаривают выделпвн 1Йс спирт И нспрореагпровавшие диметилфосфит и моноэтилальхлораль.After that, under a vacuum (30 mm Hg. Art.) And a cube temperature of 90 ° C, alcohol is distilled off from the internal liquid of 1 ° C and the unreacted dimethylphosphite and monoethyl alloral.
Отиарка считаетс закопченной, когда перестают отгон тьс летучие веш,ества. Кубовый остаток представл ет собой технический хлорофос .Otiarks are considered smoked when they stop driving away volatile substances. The bottom residue is technical chlorophos.
Выход хлорофоса 75%, содержание активного нача.ча 95%. Полученный продукт после перекристаллизации из бензола имеет т. ил. 78-79 С.The yield of chlorophos is 75%, the content of active starters is 95%. The resulting product after recrystallization from benzene has so on. Il. 78-79 C.
В случае ирименени монометилальхлорал выход хлорофоса составл ет 82%, а при использовании монобутилальхлорал - 84%.In the case of monomethylchloral, the yield of chlorophos is 82%, and when using monobutylalloral it is 84%.
Предмет изобретени Subject invention
Способ 1Юл че1П1 О,О-диметил-2,2,2-трихлор-1-оксиэт11лфосфоиата (хлорофоса) на осиове диметилфосфита, отличающийс тем, что, с целью уирошени процесса, диметилфосфиты подвергают взаимодействию с полуацеталем хлорал .Method 1 Yul che1P1 O, O-dimethyl-2,2,2-trichloro-1-hydroxyethyl phosphorous (chlorophos) on dimethyl phosphite axis, characterized in that dimethyl phosphites are reacted with helocetal hemi-acetal to erode the process.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU172326A1 true SU172326A1 (en) |
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