IP Library Granted Patent US 7,910,746
Granted Patent B2
US 7,910,746 · App. 10/597,723 · Granted Mar 22, 2011

Haloalkyl carboxamides

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Quick Facts
Patent No.
US 7,910,746
App. No.
10/597,723
Granted
Mar 22, 2011
Kind
B2
Abstract

New haloalkyl carboxamides of formula (I) in which R, R 1 , R 2 , R 3 , R 4 , M and A have the meanings specified in the description, several processes for synthesizing these materials and their use in combating undesirable microorganisms, as well as new intermediate products and their synthesis.

Claims (61)

1. A haloalkyl carboxamide of the formula (I)

in which

R stands for hydrogen or halogen,

R 1 stands for hydrogen or methyl,

R 2 stands for methyl, ethyl or C 1 -C 4 haloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms,

R 3 stands for halogen or C 1 -C 4 haloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms,

R 4 stands for hydrogen, C 1 -C 8 alkyl, C 1 -C 6 alkylsulfinyl, C 1 -C 6 alkylsulfonyl, C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl, C 3 -C 8 cycloalkyl; C 1 -C 6 haloalkyl, C 1 -C 4 haloalkylthio, C 1 -C 4 haloalkylsulfinyl, C 1 -C 4 haloalkylsulfonyl, halo-C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl, C 3 -C 8 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case; formyl, formyl-C 1 -C 3 -alkyl, (C 1 -C 3 alkyl)carbonyl-C 1 -C 3 -alkyl, (C 1 -C 3 alkoxy)carbonyl-C 1 -C 3 -alkyl; halo-(C 1 -C 3 alkyl)carbonyl-C 1 -C 3 -alkyl, halo-(C 1 -C 3 alkoxy)carbonyl-C 1 -C 3 -alkyl with 1 to 13 fluorine, chlorine and/or bromine atoms in each case; (C 1 -C 8 alkyl)carbonyl, (C 1 -C 8 alkoxy)carbonyl, (C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl)carbonyl, (C 3 -C 8 cycloalkyl)carbonyl; (C 1 -C 6 haloalkyl)carbonyl, (C 1 -C 6 haloalkoxy)carbonyl, (halo-C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl)carbonyl, (C 3 -C 8 halocycloalkyl)carbonyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case; or —C(═O)C(═O)R 5 , —CONR 6 R 7 or —CH 2 NR 8 R 9 ,

R 5 stands for hydrogen, C 1 -C 8 alkyl, C 1 -C 8 alkoxy, C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl, C 3 -C 8 cycloalkyl; C 1 -C 6 haloalkyl, C 1 -C 6 haloalkoxy, halo-C 1 -C 4 -alkoxyl-C 1 -C 4 -alkyl, C 3 -C 8 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case,

R 6 and R 7 stand independently of one another in each case for hydrogen, C 1 -C 8 alkyl, C 1 -C 4 alkoxyl C 1 -C 4 allyl, C 3 -C 8 cycloalkyl; C 1 -C 8 haloalkyl, halo-C 1 -C 4 -alkoxy-C 1 -C 4 alkyl, C 3 -C 8 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case, or

R 6 and R 7 , together with the nitrogen atom to which they are bound, form a substituted, saturated heterocycle with 5 to 8 ring atoms, with single or multiple, the same or different substitution by halogen or C 1 -C 4 alkyl, whereby the heterocycle optionally contains 1 or 2 additional, non-adjacent hetero atoms constituted of oxygen, sulfur or NR 10 ,

R 8 and R 9 stand independently of one another for hydrogen, C 1 -C 8 -alkyl, C 3 -C 8 cycloalkyl; C 1 -C 8 haloalkyl, C 3 -C 8 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case, or

R 8 and R 9 , together with the nitrogen atom to which they are bound, form a substituted, saturated heterocycle with 5 to 8 ring atoms, with single or multiple, the same or different substitution by halogen or C 1 -C 4 alkyl, whereby the heterocycle optionally contains 1 or 2 additional, non-adjacent hetero atoms constituted of oxygen, sulfur or NR 10 ,

R 10 stands for hydrogen or C 1 -C 6 alkyl,

M stands in each case for a phenyl ring with a single substitution by R 11 ,

R 11 stands for hydrogen, fluorine, chlorine, methyl, isopropyl, methylthio or trifluoromethyl,

A stands for the group of the formula (A1)

in which

R 12 stands for hydrogen, cyano, halogen, nitro, C 1 -C 4 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 alkylthio, C 3 -C 6 cycloalkyl, haloalkyl, C 1 -C 4 haloalkoxy or C 1 -C 4 haloalkylthio, in each case with 1 to 5 halogen atoms, aminocarbonyl or aminocarbonyl-C 1 -C 4 -alkyl,

R 13 stands for hydrogen, halogen, cyano, C 1 -C 4 alkyl, C 1 -C 4 alkoxy or C 1 -C 4 alkylthio, and

R 14 stands for hydrogen, C 1 -C 4 alkyl, hydroxy-C 1 -C 4 alkyl, C 2 -C 6 alkenyl, C 3 -C 6 cycloalkyl, C 1 -C 4 -alkylthio-C 1 -C 4 -alkyl, C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl, C 1 -C 4 haloalkyl, C 1 -C 4 -haloalkylthio-C 1 -C 4 -alkyl, C 1 -C 4 -haloalkoxy-C 1 -C 4 -alkyl in each case with 1 to 5 halogen atoms, or phenyl.

2. A haloalkyl carboxamide of the formula (I) according to claim 1 , in which

R stands for hydrogen, fluorine, chlorine or bromine,

R 1 stands for hydrogen or methyl,

R 2 stands for methyl, ethyl or in each case for methyl, ethyl, n- or isopropyl, n-, iso-, sec- or tert-butyl with single or multiple, the same or different, substitution by fluorine, chlorine or bromine,

R 3 stands for fluorine, chlorine, bromine, iodine or in each case for methyl, ethyl, n- or isopropyl, n-, iso-, sec- or tert-butyl with single or multiple, the same or different, substitution by fluorine, chlorine or bromine,

R 4 stands for hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylsulfinyl, C 1 -C 4 alkylsulfonyl, C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl, C 3 -C 6 cycloalkyl; C 1 -C 4 haloalkyl, C 1 -C 4 haloalkylthio, C 1 -C 4 haloalkylsulfinyl, C 1 -C 4 haloalkylsulfonyl, halo-C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl, C 3 -C 8 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case; formyl, formyl-C 1 -C 3 -alkyl, (C 1 -C 3 alkyl)carbonyl-C 1 -C 3 -alkyl, (C 1 -C 3 alkoxy)carbonyl-C 1 -C 3 -alkyl; halo-(C 1 -C 3 alkyl)carbonyl-C 1 -C 3 -alkyl, halo-(C 1 -C 3 alkoxy)carbonyl-C 1 -C 3 -alkyl with 1 to 13 fluorine, chlorine and/or bromine atoms in each case; (C 1 -C 6 alkyl)carbonyl, (C 1 -C 4 alkoxy)carbonyl, (C 1 -C 3 -alkoxy-C 1 -C 3 alkyl)carbonyl, (C 3 -C 6 cycloalkyl)carbonyl; (C 1 -C 4 haloalkyl)carbonyl, (C 1 -C 4 haloalkoxy)carbonyl, (halo-C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl)carbonyl, (C 3 -C 6 halocycloalkyl)carbonyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case; or —C(═O)C(═O)R 5 , —CONR 6 R 7 or —CH 2 NR 8 R 9 ,

R 5 stands for hydrogen, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl, C 3 -C 6 cycloalkyl; C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, halo-C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl, C 3 -C 6 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case,

R 6 and R 7 stand independently of one another in each case for hydrogen, C 1 -C 6 alkyl, C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl, C 3 -C 6 cycloalkyl; C 1 -C 4 haloalkyl, halo-C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl, C 3 -C 6 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case, or

R 6 and R 7 , together with the nitrogen atom to which they are bound, form a substituted, saturated heterocycle with 5 to 8 ring atoms, with single or multiple, the same or different substitution by halogen or C 1 -C 4 alkyl, whereby the heterocycle optionally contains 1 or 2 additional, non-adjacent hetero atoms constituted of oxygen, sulfur or NR 10 ,

R 8 and R 9 stand independently of one another for hydrogen, C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl; —C 4 haloalkyl, C 3 -C 6 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case, or

R 8 and R 9 , together with the nitrogen atom to which they are bound, form a substituted, saturated heterocycle with 5 to 8 ring atoms, with single or multiple, the same or different substitution by halogen or C 1 -C 4 alkyl, whereby the heterocycle optionally contains 1 or 2 additional, non-adjacent hetero atoms constituted of oxygen, sulfur or NR 10 ,

R 10 stands for hydrogen or C 1 -C 4 alkyl,

M stands for the following cyclic

whereby the bond marked with an asterisk (“*”) is a link with the amide, and the bond marked with “#” is a link with the haloalkyl group,

R 11 stands for hydrogen, fluorine, chlorine, methyl or trifluoromethyl,

A stands for the group of the formula (A1)

in which

R 12 stands for hydrogen, cyano, fluorine, chlorine, bromine, iodine, methyl, ethyl, isopropyl, methoxy, ethoxy, methylthio, ethylthio, cyclopropyl, C 1 -C 2 haloalkyl, C 1 -C 2 haloalkoxy in each case with 1 to 5 fluorine, chlorine and/or bromine atoms, trifluoromethylthio, difluoromethylthio, aminocarbonyl, aminocarbonylmethyl or aminocarbonylethyl,

R 13 stands for hydrogen, fluorine, chlorine, bromine, iodine, methyl, ethyl, methoxy, ethoxy, methylthio or ethylthio, and

R 14 stands for hydrogen, methyl, ethyl, n-propyl, isopropyl, C 1 -C 2 haloalkyl with 1 to 5 fluorine, chlorine and/or bromine atoms, hydroxymethyl, hydroxyethyl, cyclopropyl, cyclopentyl, cyclohexyl or phenyl.

3. A process for synthesizing a haloalkyl carboxamide of the formula (I) according to claim 1 , comprising

a) reacting a carboxylic acid derivative of the formula (II)

in which

A has the meaning as defined above in claim 1 and

X 1 stands for halogen or hydroxy,

with an aniline derivative of the formula (III)

in which

R, R 1 , R 2 , R 3 , R 4 and M have the meanings as defined above in claim 1 ,

optionally in the presence of a catalyst, optionally in the presence of a condensation agent, optionally in the presence of an acid binder and optionally in the presence of a diluent,

or

b) reacting a haloalkylcarboxanilide of the formula (I-a)

in which

R, R 1 , R 2 , R 3 , M and A have the meanings as defined above in claim 1 , with a halide of the formula (IV)

R 4-A —X 2   (IV)

in which

X 2 stands for chlorine, bromine or iodine,

R 4-A stands for C 1 -C 8 alkyl, C 1 -C 6 alkylsulfinyl, C 1 -C 6 alkylsulfonyl, C 1 -C 4 alkoxy-C 1 -C 4 alkyl, C 3 -C 8 cycloalkyl; C 1 -C 6 haloalkyl, haloalkylthio, C 1 -C 4 haloalkylsulfinyl, C 1 -C 4 haloalkylsulfonyl, halo-C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl, C 3 -C 8 halocycloalkyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case; formyl, formyl-C 1 -C 3 -alkyl, (C 1 -C 3 alkyl)carbonyl-C 1 -C 3 -alkyl, (C 1 -C 3 alkoxy)carbonyl-C 1 -C 3 -alkyl; halo-(C 1 -C 3 alkyl)carbonyl-C 1 -C 3 -alkyl, halo-(C 1 -C 3 alkoxy)carbonyl-C 1 -C 3 -alkyl with 1 to 13 fluorine, chlorine and/or bromine atoms in each case; (C 1 -C 8 alkyl)carbonyl, (C 1 -C 8 alkoxy)carbonyl, (C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl)carbonyl, (C 3 -C 8 cycloalkyl)carbonyl; (C 1 -C 6 haloalkyl)carbonyl, (C 1 -C 6 haloalkoxy)carbonyl, (halo-C 1 -C 4 -alkoxy-C 1 -C 4 -alkyl)carbonyl, (C 3 -C 8 halocycloalkyl)carbonyl with 1 to 9 fluorine, chlorine and/or bromine atoms in each case; or —C(═O)C(═O)R 5 , —CONR 6 R 7 or —CH 2 NR 8 R 9 , whereby R 5 , R 6 , R 7 , R 8 and R 9 have the meanings as defined above in claim 1 ,

in the presence of a base and a dilution medium.

4. A composition for combating undesirable microorganisms, comprising at least one haloalkyl carboxamide of the formula (I) according to claim 1 together with extenders and/or surface-active materials.

5. A method for combating undesired microorganisms, comprising applying at least one haloalkyl carboxamide of the formula (I) according to claim 1 to the microorganisms and/or their environment.

6. A method for preparing a composition to combat undesired microorganisms, comprising mixing at least one haloalkyl carboxamide of the formula (I) according to claim 1 with extenders and/or surface-active materials.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 20, 2015
From: BAYER CROPSCIENCE AG
To: BAYER INTELLECTUAL PROPERTY GMBH
Reel/Frame 034990/0879 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 11, 2007
From: DUNKEL, RALF; ELBE, HANS-LUDWIG; HARTMANN, BENOIT; GREUL, JORG NICO; ILG, KERSTIN; WACHENDORF-NEUMANN, ULRIKE; DAHMEN, PETER; KUCK, KARL-HEINZ
To: BAYER CROPSCIENCE AG
Reel/Frame 019813/0204 →