IL33504A - The production of esters and amides of o-(-2-bromoethyl)-o-(2,2-dichlorovinyl)-phosphoric acid,and pesticidal compositions containing such compounds - Google Patents

The production of esters and amides of o-(-2-bromoethyl)-o-(2,2-dichlorovinyl)-phosphoric acid,and pesticidal compositions containing such compounds

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Publication number
IL33504A
IL33504A IL33504A IL3350469A IL33504A IL 33504 A IL33504 A IL 33504A IL 33504 A IL33504 A IL 33504A IL 3350469 A IL3350469 A IL 3350469A IL 33504 A IL33504 A IL 33504A
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IL
Israel
Prior art keywords
compound
carbon atoms
formula
alkyl
admixture
Prior art date
Application number
IL33504A
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IL33504A0 (en
Original Assignee
Bayer Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Bayer Ag filed Critical Bayer Ag
Publication of IL33504A0 publication Critical patent/IL33504A0/en
Publication of IL33504A publication Critical patent/IL33504A/en

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/547Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
    • C07F9/6564Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
    • C07F9/6571Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
    • C07F9/657154Cyclic esteramides of oxyacids of phosphorus
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/08Esters of oxyacids of phosphorus
    • C07F9/09Esters of phosphoric acids
    • C07F9/113Esters of phosphoric acids with unsaturated acyclic alcohols
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/16Esters of thiophosphoric acids or thiophosphorous acids
    • C07F9/165Esters of thiophosphoric acids
    • C07F9/173Esters of thiophosphoric acids with unsaturated acyclic alcohols
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/22Amides of acids of phosphorus
    • C07F9/24Esteramides
    • C07F9/2404Esteramides the ester moiety containing a substituent or a structure which is considered as characteristic
    • C07F9/2412Esteramides the ester moiety containing a substituent or a structure which is considered as characteristic of unsaturated acyclic alcohols

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

The present invention relates to an unobvious process for the production of insecticidal acid esters or and to some of these pounds which are Prom German Patent Specification it is known that dioxaphospholanes can be reacted with chloral to give acid in German Published Specification 1 232 961 there is already described a process for the preparation of esters of some acids of phosphorus which among other things but in a completely different way to acid It has now been found that the analogously structured bromoethy acid compounds of the general formula R 0 i in which R stands for alkoxyalkyl or and X stands for dialkylamino alkylarylamino or can be prepared in high yield and purity by a process in which of the general formula ο t In this connection it is most surprising and unexpected that only the bromine atom causes the splitting of the pholane ring and enters the newly formed Since as stated in the German patent specification mentioned brings about the ring splitting described with the same ease in exothermal it was to have been expected that the use of bromodichloroacetaldehyde instead of chloral would give a mixed product in which bromine and chlorine atoms are distributed stically between the haloalkyl and the dihalovinyl is not the The products of the process according to the invention are homogeneous and correspond to the general formula as can be proved for example by nuclear resonance the process according to the measured against the prior represents an If and dehyde are used as starting the reaction can be esented by the following reaction The to be used as starting materials are generally defined by the above formula In formulae and it is preferred that stands for alkyl or haloalkyl with carbon alkoxyalkyl with carbon or alkenoxyalkyl with 3 to 6 carbon and X for alkoxy or with carbon lower As examples of the of formula which can be used according to the the following may be hospholane thio allyloxy The compounds of formula are known and can be produced even on an industrial The reaction may be carried out in the presence of a 5 such as benzene and ohlorlnated aliphatic such as and and suoh as diethyl In the reaction be carried out without a The reaction temperatures can be varied within a fairly wide In the work is carried out at from 0 to preferably 30 to The reaction is and temperature oan be regulated by addition of the aldehyde of the formula For the carrying out of the process aocording to the the desired of the formula may be dissolved in one of the solvents mentioned and the amount of of the formula may be added For working the reaotion solutions are washed dried and Many of the products so obtained can be purified by Where this is not possible because of the risk of the crude products may be under greatly reduoed from residues of The substanoes obtainable according to the process of the invention for the most and are used as The invention also provides a pesticidal composition ontaining as active ingredient a compound produced by a process according to the invention in admixture with a liquid diluent or carrier containing a active The diluent or carrier may be any of those known to the The composition generally contains to 90 by weight of the and may be diluted for actual The invention also provides a method of combating Le A 11931 5a cultural peata which comprisee to the peats or a habitat thereof a compound according to the invention or produced by a process according to the invention alone or in the form of a composition containing as aotive ingredient the compound in mixture with a solid or liquid diluent or The invention also provides crops protected from damage by pests by being grown in areas in prior to or during the time of the a compound according to the invention or produced by a process according to the invention was applied alone or in admixture with a solid or liquid diluent or The process of the and the pesticidal activity of the are illustrated by the following Example 1 0 48 g 25 are added with to 5 g pholane in 200 ml The temperature rises to Stirring is continued for two to three the temperature falling again to room The reaction mixture is washed neutral with dried over sodium filtered off and For the oily residue can be obtained as colourless oil of boiling point Hg and the refractive index g of the Calculated for 9 Example 2 0 The compound is prepared analogously to that of Example 1 from pro and propyl phosphoric acid ester is obtained as a colourless oil of boiling point mm Hg and the refractive index of the theory Calculated for Example 3 The compound is prepared analogously to Example 1 from and acid ester is obtained as yellow oil of boiling point 3 mm Hg and the refractive index Yield of the theory Analysis P S Calculated for Example 4 0 The compound is prepared analogously to Example 1 from and h l l Hg and refractive index of the theory Calculated for The compound is prepared analogously to Example 1 from and acid amide is obtained as colourless oil of boiling point mm Hg and the refractive index of the theory N P Calculated for Example 6 Q The compound is prepared analogously to Example 1 from and acid amide is obtained as colourless oil of boiling point mm Hg and the refractive index of the theory N P Calculated for Example 7 The compound prepared analogously to Example 1 from and acid ester is obtained as yellowish oil of boiling point mm Hg and the tive index of the Calculated for Example 8 The compound is prepared analogously to Example 1 from and but stirring is effected at 50 to acid ester is obtained oil of refractive index of the theory Analysi Calculated for Example 9 The prepared analogously to Example 1 from and acid eater is obtained as yellow oil of 21 refractive index of the theory Calculated for Example The compound is prepared analogously to Example 1 from and acid ester is obtained as yellow oil of refractive index of the theory Calculated for Le A 10 Example A Teat Aedes aegypti Solven Acetone 2 parts by weight of active compound are dissolved in 1000 parts by volume of The solution so obtained is diluted with further solvent to the desired lower ml of the solution of active compound are pipetted into a Petri On the bottom of the Petri dish there is a filter paper with a diameter of about The Petri dish remains uncovered until the solvent has completely The amount of active compound per square metre of filter paper varies with the concentration of the solution of active compound About 25 test animals are then placed in the Petri dish and it is covered with a glass The condition of the test animals is continuously The time which is necessary for a knock down effect is The test the active the concentrations of the active compounds and the periods of time at which there is a knock down effect can be from Table Table A Active compounds Concentrations of active compound solution 0 2 5 A 11931 12 Example B Test domestiea Solven Acetone 2 parte by weight of active compound are dissolved in 1000 parts by volume of The solution so obtained is diluted with further solvent to the desired lower ml of the solution of active compound are pipetted into a Petri On the bottom of the Petri dish there is a ter paper with a diameter of about The Petri dish remains uncovered until the solvent has completely The amount of active compound per square metre of filter paper varies with the concentration of the solution of active compound About 25 test animals are then placed in the Petri dish and it is covered with a glass The condition of the test animals is continuously The time which is necessary for a knock down effect is The test the active the concentrations of the active compounds and the periods of time at whioh there is a knock down effect can be seen from Table Table B for Dlptera Ac ive compounds Concentrations of active compound solution Example G Teat animals Sitophilua granarius Solven Acetone 2 parts by weight of the active compound are dissolved in 1000 parts by volume of the The solution so obtained is diluted with further solvent to the desired concentrations ml of the solution of the active compound are pipetted into a Petri On the bottom of the Petri dish there is a filter paper with a diameter of about The Petri dish mains uncovered until the solvent has completely The amount of active compound per square metre of filter paper varies with the concentration of the solution of active compound About 25 test animals are then placed in the Petri dish and it is oovered with a glass The condition of the test animals is observed after 1 and 3 days after the commencement of the The knock down effect is determined as a The active the concentratio s of the active the test animals and the results can be seen from Table Table AotiTe compounda Concentrations of Destruction compound in 0 100 30 insufficientOCRQuality

Claims (15)

WHIT WE CLAIM IS:-
1. A prooess for the production of a 2- acid ester or amide of the formula H 0 Br-CH2-CH-0-P-0-CH=0Cl2 (I ) X in which H stands for hydrogen, alkyl, haloalkyl, alkoxyalkyl or alkenoxyalkyl, and .thio X stands for alkoxy, aryloxy, alkylaryloxy, alkylAercapto , .thio arylaegeapte, dialkylamino, dialkenylamino, diarylamino, alkylarylamino or T-alkyl-2-alkoxycarbonyl7-vinyloxy in which a 1, 3»2-dioxaphospholane of the general formula is reacted with bromodichloroacetaldehyde of the formula CI 0 Br-C- C (III) t I CI H
2. A process according to claim 1 in which R stands for alkyl or haloalkyl with 1-4 carbon atoms, alkoxyalk l with 2-6 carbon atoms, or alkenoxyalkyl with 3 to 6 carbon atoms; and X for alkoxy or alkylaeseep-*©- with 1-4 carbon atoms, £L-methyl-2-ethoxycarbonyl /thio -vinyl-oxy, phenoxy, lower alkylphenyloxy, phenylmei-aap e^ dialkylamino with 2-8 carbon atoms, dialkenylamino with 4-8 carbon atoms, diphenylamino, or N-alkyl-N-arylamino, especially N-lower-alkyl-N-phenylamino.
3. A process according to claim 1 or 2 in which the compound of formula (II) is one of those hereinbefore listed.
A rooess aooordin to an of claims 1-3 in which the reac 33504/2 - 18 -
5. A process aocording to claim 4 in hiob the solvent is one of those hereinbefore mentioned.
6. -A prooeas acoording to any of. olaima 1-5 in hioh the reaction ia carried out at 0 to 100°C.
7. A prooesa according to claim 6 in whioh the reaotion ia oarried out at 30 to 70°C.
8. A prooesa acoording to any of claims 1-7 in whioh the compound of the formula (II) ia dissolved in a solvent and an equimolar amount of bromodiohloroacetaldehyde ia added dropwiae.
9. A prooeas aocording to olaim 1, substantially as hereinbefore described in any of Examples 1-10.
10. 0- 2-bromoethy3 -0-^,2-diohlorovinyl7-pbosphorio acid eaters and amides as defined in olaim 1, whenever prepared by a process acoording to any of claims 1-9.
11. Gompounds hereinbefore identified as (4), (9) and (10) whenever prepared by a process according to any of Claims 1-9.
12. A pesticidal composition containing as active ingredient a compound according to Claim 10 or 11 in admixture with a solid diluent or carrier or in admixture with a liquid diluent or carrier containing a surface-active agent.
13. A composition a ccording to Claim 12 containing from 0.1 to 5$ of the active compound by weight.
14. A method of combating agricultural pests which comprises applying to the pests or a habitnt thereof a compoind according to Claim 10 or 11 alone or in the form of a composition containing as active ingredient a compound according to Claim 10 or 11 in admixture with a solid or liquid diluent or carrier. 33504/2 19
15. Crops protected from daaaage by being grown in areas in which, imnediately prior to and/or during the time of the growing, a compound according to any of Claims 10 or 11 was applied alone or in admixture with a solid or liquid diluent or carrier. ND:BH
IL33504A 1968-12-24 1969-12-09 The production of esters and amides of o-(-2-bromoethyl)-o-(2,2-dichlorovinyl)-phosphoric acid,and pesticidal compositions containing such compounds IL33504A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1816903A DE1816903C3 (en) 1968-12-24 1968-12-24 0- [2-bromoethyl] - 0 - [2,2-dichloro-vinyl] phosphoric acid ester !! or amides, process for their production

Publications (2)

Publication Number Publication Date
IL33504A0 IL33504A0 (en) 1970-02-19
IL33504A true IL33504A (en) 1972-12-29

Family

ID=5717339

Family Applications (1)

Application Number Title Priority Date Filing Date
IL33504A IL33504A (en) 1968-12-24 1969-12-09 The production of esters and amides of o-(-2-bromoethyl)-o-(2,2-dichlorovinyl)-phosphoric acid,and pesticidal compositions containing such compounds

Country Status (14)

Country Link
AT (1) AT291296B (en)
BE (1) BE743707A (en)
BG (1) BG17012A3 (en)
CH (1) CH533641A (en)
CS (1) CS158659B2 (en)
DE (1) DE1816903C3 (en)
DK (1) DK122967B (en)
ES (1) ES374846A1 (en)
FR (1) FR2027083A1 (en)
GB (1) GB1243599A (en)
IL (1) IL33504A (en)
NL (1) NL6919029A (en)
RO (1) RO56628A (en)
YU (1) YU316069A (en)

Also Published As

Publication number Publication date
DK122967B (en) 1972-05-01
CH533641A (en) 1973-02-15
FR2027083A1 (en) 1970-09-25
AT291296B (en) 1971-07-12
DE1816903B2 (en) 1977-09-22
ES374846A1 (en) 1972-01-16
BE743707A (en) 1970-06-24
RO56628A (en) 1974-09-01
CS158659B2 (en) 1974-11-25
NL6919029A (en) 1970-06-26
GB1243599A (en) 1971-08-18
YU316069A (en) 1978-10-31
DE1816903C3 (en) 1978-05-24
BG17012A3 (en) 1973-04-25
DE1816903A1 (en) 1970-07-16
IL33504A0 (en) 1970-02-19

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