[go: up one dir, main page]

IE32444B1 - (-) (cis-1,2-epoxypropyl)phosphonic acid derivatives - Google Patents

(-) (cis-1,2-epoxypropyl)phosphonic acid derivatives

Info

Publication number
IE32444B1
IE32444B1 IE1253/68A IE125368A IE32444B1 IE 32444 B1 IE32444 B1 IE 32444B1 IE 1253/68 A IE1253/68 A IE 1253/68A IE 125368 A IE125368 A IE 125368A IE 32444 B1 IE32444 B1 IE 32444B1
Authority
IE
Ireland
Prior art keywords
salt
epoxypropyl
cis
phosphonic acid
reacting
Prior art date
Application number
IE1253/68A
Other versions
IE32444L (en
Original Assignee
Merck & Co Inc
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.)
Filing date
Publication date
Application filed by Merck & Co Inc filed Critical Merck & Co Inc
Publication of IE32444L publication Critical patent/IE32444L/en
Publication of IE32444B1 publication Critical patent/IE32444B1/en

Links

Classifications

    • 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
    • C07F9/655Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms
    • C07F9/65502Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms the oxygen atom being part of a three-membered ring
    • C07F9/65505Phosphonic acids containing oxirane groups; esters thereof

Landscapes

  • 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)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

1,239,986. (-)(Bis - 1,2 - epoxypropyl)phosphonic acid derivatives. MERCK & CO. Inc. 24 Oct., 1968 [15 May, 1968; 28 Aug., 1968], No. 50631/68. Heading C2C. [Also in Division A5] The invention comprises (a) esters of (-)(cis- 1,2 - epoxypropyl)phosphonic acid of the formula wherein R is a substituted or unsubstituted hydrocarbyl or heterocyclic group, R 1 is H or an equivalent of a salt-forming cation, or a substituted or unsubstituted hydrocarbyl or heterocyclic group or R and R 1 together form a hydrocarbylene e.g. methylene, ethylene, propylene or arylene bridge, and (b) derivatives of (-) (cis - 1,2 - epoxypropyl)phosphonic acid of the formula in which Y is an -OR 2 group or a halogen atom where R 2 is C 1 -C 6 alkyl, C 1 -C 6 substituted alkyl, C 2 -C 6 alkenyl, C 2 -C 6 alkynyl, aryl, substituted aryl, aralkyl, or substituted aralkyl and Y<SP>1</SP> is a halogen atom. The hydrocarbyl or substituted hydrocarbyl radicals may be substituted or unsubstituted alkyl radicals, or alkenyl, alkynyl, cycloaliphatic, araliphatic or aromatic radicals. The esters (I) may be prepared (a) by reacting a heavy metal (preferably silver) salt of (-)(cis - 1,2 - epoxypropyl)phos. phonic acid with a halide (R Hal); (b) by reacting the free phosphonic acid with a diazoalkane or diazoaralkane, (c) by reacting (-)(cis - 1,2- epoxypropyl)phosphonic dichloride with an alcohol or phenol (ROH) conveniently in the presence of a tertiary amine, this reaction being operable to prepare mono- or di-esters by using appropriate molar proportions of the reactants, (d) by reacting a salt of the phosphonic, e.g. an alkali metal or amine salt with an alcohol or thiol in the presence of an activating agent e.g. a carbodiimide such as dicyclohexyl carbodiimide, an arylsulphonyl halide, e.g. 2,4,6- trimethylsulphonyl chloride or trichloroacetonitrile. Monoesters may also be obtained by reacting a diester with a dilute base e.g. NaOH or KOH at a pH of 8-13 to remove one ester residue. Mixed esters may be prepared (a) by reacting a (-)(cis - 1,2 - epoxypropyl)monoester phosphonohalidate with an alcohol or thiol in the presence of an acid binding agent, e.g. a tertiary amine, or (b) by converting a monoester mono-alkali metal salt to the free acid and then to the mono-silver salt by reaction with a soluble silver salt and then reacting the monosilver salt monoester with a hydrocarbyl halide the hydrocarbon residue of which is different from that of the monoester radical. Diesters may also be obtained by treatment of a 1 - chloro - 2- hydroxypropyl phosphonic acid diester with a base. The (-)(cis - 1,2 epoxypropyl)phosphonic dihalides may be obtained by reacting the free phosphonic acid with a halogenating agent, preferably a thionyl halide such as thionyl chloride. The ester and ester salt products have antibacterial properties and the diester products may be converted to monoamide derivatives of (-)(cis - 1,2 - epoxypropyl)phosphonic acid salts thereof, e.g. by hydrolysing with alkali to form a monoester which is reacted with thionyl chloride to form the monoester chloride, the latter being then reacted with an amine to form the monoester monoamide which on hydrolysis with an alkali, e.g. NaOH, forms a salt of the monoamide. The diesters may be converted to the free phosphonic acid or salts thereof by various methods e.g. as disclosed in Specification No. 1,236,955/68. Di - n - butyl cis propenylphosphonate is obtained by hydrogenation of di - n - butyl propynyl phosphonate and is converted to cispropenyl phosphonic acid by treatment with concentrated HC1 followed by the addition of water and the free acid after neutralization with NB 4 OH to pH 5À5 is epoxidized to form the ammonium salt of, (Œ)(cis - 1,2 - epoxypropyl)- phosphonic acid which is then resolved by use of (+ )α - phenethylamine to form the (+)α- phenylethylamine salt of (-)(cis - 1,2 - epoxypropyl)phosphonic acid from which the free phosphonic acid is obtained by passing a solution of the salt over an ion exchange resin on the H<SP>+</SP> cycle. Di - n - butyl propynylphosphonate is obtained by reacting methylacetylene magnesium bromide with di - n - butyl chlorophosphonate, a detailed example being given. [GB1239986A]
IE1253/68A 1968-05-15 1968-10-21 (-) (cis-1,2-epoxypropyl)phosphonic acid derivatives IE32444B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US72944468A 1968-05-15 1968-05-15
US75580568A 1968-08-28 1968-08-28

Publications (2)

Publication Number Publication Date
IE32444L IE32444L (en) 1969-11-15
IE32444B1 true IE32444B1 (en) 1973-08-08

Family

ID=27111879

Family Applications (1)

Application Number Title Priority Date Filing Date
IE1253/68A IE32444B1 (en) 1968-05-15 1968-10-21 (-) (cis-1,2-epoxypropyl)phosphonic acid derivatives

Country Status (14)

Country Link
AT (3) AT299246B (en)
BE (1) BE723075A (en)
BG (1) BG16345A3 (en)
CH (1) CH537953A (en)
ES (1) ES359543A1 (en)
FR (1) FR2008585B1 (en)
GB (1) GB1239986A (en)
HU (1) HU163312B (en)
IE (1) IE32444B1 (en)
IL (1) IL30921A0 (en)
LU (1) LU57188A1 (en)
MT (1) MTP594B (en)
NL (1) NL6814984A (en)
ZM (1) ZM14368A1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL6814984A (en) * 1968-05-15 1969-11-18

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL6814984A (en) * 1968-05-15 1969-11-18

Also Published As

Publication number Publication date
BG16345A3 (en) 1972-08-20
FR2008585B1 (en) 1973-12-21
AT294120B (en) 1971-11-10
BE723075A (en) 1969-04-29
CH537953A (en) 1973-06-15
AT299247B (en) 1972-06-12
ES359543A1 (en) 1970-08-16
HU163312B (en) 1973-07-28
ZM14368A1 (en) 1970-06-18
FR2008585A1 (en) 1970-01-23
LU57188A1 (en) 1969-05-16
MTP594B (en) 1971-04-14
IE32444L (en) 1969-11-15
NL6814984A (en) 1969-11-18
GB1239986A (en) 1971-07-21
IL30921A0 (en) 1968-12-26
DE1805682A1 (en) 1969-12-11
AT299246B (en) 1972-06-12

Similar Documents

Publication Publication Date Title
GB1140980A (en) New diphosphonic acids, derivatives thereof and detergent compositions containing them
DE59906738D1 (en) Process for the preparation of phosphinic acid esters
IE40852L (en) Fungicidal phosphonates
DE50104089D1 (en) Process for the preparation of ethane-1,2-bis (alkylphosphinic acids)
US2903475A (en) Production of esters of phosphonous and phosphinous acids
DE69331314D1 (en) Process for the preparation of N-phosphonomethyliminodiacetic acid
FI894127A0 (en) Process for Continuous Preparation of 2-Phosphonobutane-1,2,4-Tricarboxylic Acid and Its Alkali Metal Salts
IE32444B1 (en) (-) (cis-1,2-epoxypropyl)phosphonic acid derivatives
GB1265167A (en)
GB1075125A (en) Improvements relating to phosphorus-containing metal-organic compounds
ATE248180T1 (en) METHOD FOR PRODUCING PHOSPHONIC ACID ESTERS
US3271481A (en) 2, 6-disubstituted primary aryl phosphites and phosphorodihalidites and processes for the manufacture thereof
ATE20668T1 (en) PROCESS FOR THE PREPARATION OF ALKALI METAL SALTS OF 1-PHOSPHONOPROPANE-1,2,3-TRICARBONIC ACID.
EP0061106A3 (en) Process for preparing oligophosphonic acids or oligophosphinic acids, their salts and/or esters, as well as phosphonic and phosphinic acid derivatives
GB1274350A (en) 2-chloroethane-(thiono)-phosphonic acid derivatives, process for their preparation, and their use for the regulation of plant growth
GB934090A (en) Chloromethylphosphinic acid, salts thereof, and method of preparation
ATE3404T1 (en) PROCESS FOR THE PREPARATION OF 1,1-DIHALOGENALKENES.
GB1398844A (en) Manufacture of 1-hydroxyethane 1,1-diphosphonic acid
GB702750A (en) Synthesis of pantothenic acid-4 phosphate
DE2846835A1 (en) METHOD FOR PRODUCING CARBOXYLALKANE-AMINOALKANE DIPHOSPHONIC ACIDS AND AMINOARYLALKANE DIPHOSPHONIC ACIDS
ES367106A1 (en) Preparation of (cis-1,2-epoxypropyl)phosphonic acid and its salts and esters
US3007952A (en) Organo-phosphorus compounds and preparation
KR910018392A (en) Process for preparing phosphono organo carboxylic acid
GB1512185A (en) Process for conditioning fibres and heat-resistant fibre-conditioning agents therefor
GB1212931A (en) Phosphorus compounds containing phosphorus to carbon linkages