SU545647A1 - Method for preparing 0,0-dimethyl-0-2, 2-dichlorovinyl phosphate - Google Patents
Method for preparing 0,0-dimethyl-0-2, 2-dichlorovinyl phosphateInfo
- Publication number
- SU545647A1 SU545647A1 SU2142804A SU2142804A SU545647A1 SU 545647 A1 SU545647 A1 SU 545647A1 SU 2142804 A SU2142804 A SU 2142804A SU 2142804 A SU2142804 A SU 2142804A SU 545647 A1 SU545647 A1 SU 545647A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dimethyl
- preparing
- chlorophos
- dichlorovinyl phosphate
- water
- Prior art date
Links
- OEBRKCOSUFCWJD-UHFFFAOYSA-N dichlorvos Chemical compound COP(=O)(OC)OC=C(Cl)Cl OEBRKCOSUFCWJD-UHFFFAOYSA-N 0.000 title description 3
- 229960001952 metrifonate Drugs 0.000 description 7
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Description
веж8ства94-96%. Хлорофос в целевом продукте отсутствует.Wells494-96%. Chlorophos in the target product is missing.
Пример. К 500 г 24,2%-ного раствора технического хлорофоса в воде в присутствии 194 г толуола при непрерывном эффек- тивном перемешивании добавл ют в течение 30 мин 232 МП 25%-ного раствора едкого натра до значени рН 10,2. По окончании дозировки щелочи реакционную массу обрабатывают 16мл 27%-ной сол ной кислоты до значени рН 4. Полученную реакционную массу раздел ют, органический слой промывают водой в объемном соотношении 1:1, отгон ют растворитель и получают 88,3 г ДДВФ с содержанием действующего начала 94,2%. Example. To 500 g of a 24.2% solution of technical chlorophos in water in the presence of 194 g of toluene, with continuous effective stirring, 232 MP of a 25% aqueous solution of sodium hydroxide are added over 30 minutes to a pH value of 10.2. At the end of the alkali dosage, the reaction mass is treated with 16 ml of 27% hydrochloric acid to a pH of 4. The resulting reaction mass is separated, the organic layer is washed with water in a 1: 1 volume ratio, the solvent is distilled off and 88.3 g of DDVF are obtained with the active content start 94.2%.
Выход 79,7%, хлорофос отсутствуетOutput 79.7%, no chlorophos
о,about,
: 1,421 - П ° : 1,4540: 1,421 - П °: 1,4540
П р и м е р 2. К 1ООО г 15,8%-ного раствора хлорофоса в присутствии 250 г ксилола при непрерьшном эффективном перемешивакии добавл ют в течение 40 мин 228 мл раствора едкого натра до значени рН 9,7. По окончании дозировки реакционную массу обрабатывают 5,5 мл концентрированной серной кислоты до значе- НИЛ рН 1. После водной промывки и отгонки растворител (аналогично прш :еру 1} получают 115 г ДДВФ с содержанием действук дцего начала 96,1%.EXAMPLE 2. To 1OOO g of a 15.8% solution of chlorophos in the presence of 250 g of xylene with continuous effective stirring, 228 ml of sodium hydroxide solution are added over 40 minutes to a pH of 9.7. At the end of the dosage, the reaction mass is treated with 5.5 ml of concentrated sulfuric acid to a NIL pH 1. After water washing and distilling off the solvent (similarly as: 1), 115 g of DDVF with an active content of 96.1% are obtained.
Выход 81,3%, хлорофос отсутствует.Yield 81.3%, chlorophos is absent.
П р и м е р 3. В реактор загружают НООг маточника со стадии получени кристаллического хлорофоса, содержащего 7,85%Example 3: The HOOg liquor from the stage of the preparation of crystalline chlorophos containing 7.85% was charged to the reactor.
монометилфосфористой и фосхл орехи ОС а, 1;monomethylphosphorous and foskhl nuts OS a, 1;
фористой кислот и 10,9 аммонийных солей вышеуказанных кислот, 155мл толуола и при интенсивном перемешивании и температуре 30°С дозируют 214 г 25%-ного раствора щелочи в течение 60 мин. По окончайии дозировки щелочи в реактор ввод т 210 мл кислых вод с системы получени пиметслфосфита до рН 4,0 и после 10 мин перемешивани отдел ют водный слой от органической фазы.foric acids and 10.9 ammonium salts of the above acids, 155 ml of toluene and with vigorous stirring and at a temperature of 30 ° C dispense 214 g of a 25% aqueous solution of alkali within 60 minutes. At the end of the alkali dosage, 210 ml of acidic water was introduced into the reactor from the pimethsphosphite production system to pH 4.0, and after 10 minutes of stirring, the aqueous layer was separated from the organic phase.
Органический слой промывают 10О мл воды и азеотропной сушкой выдел ют 54,2г ДДВФ с содержанием основного вещества 95%.The organic layer was washed with 10 O ml of water and 54.2 g of HDF with a 95% content of the basic substance were azeotropically dried.
Выход 67,4%. Хлорофос отсутствует.Yield 67.4%. Chlorophos is absent.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2142804A SU545647A1 (en) | 1975-06-11 | 1975-06-11 | Method for preparing 0,0-dimethyl-0-2, 2-dichlorovinyl phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2142804A SU545647A1 (en) | 1975-06-11 | 1975-06-11 | Method for preparing 0,0-dimethyl-0-2, 2-dichlorovinyl phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU545647A1 true SU545647A1 (en) | 1977-02-05 |
Family
ID=20622224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU2142804A SU545647A1 (en) | 1975-06-11 | 1975-06-11 | Method for preparing 0,0-dimethyl-0-2, 2-dichlorovinyl phosphate |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU545647A1 (en) |
-
1975
- 1975-06-11 SU SU2142804A patent/SU545647A1/en active
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