- Synthesis method for improving purity of fluorochloridone
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The invention discloses a synthesis method for improving the purity of fluorochloridone, and belongs to the technical field of pesticide intermediates. The synthesis method comprises the following steps: S1, taking a compound shown as a formula (III) and allyl chloride as raw materials, taking an alkaline solution or a salt solution as a solvent, carrying out catalytic reaction at 20-25 DEG C under the action of a phase transfer catalyst, and treating after the reaction is finished to obtain a compound shown as a formula (II); S2, taking the compound as shown in the formula (II) as a raw material, taking anhydrous 1, 2-dichloroethane as a solvent, and carrying out reflux reaction at 80-100 DEG C for 4-6 hours under the combined catalytic action of cuprous chloride and 2, 2-dipyridyl, so as to prepare a mixture containing fluorochloridone; and S3, purifying the fluorochloridone. During purification, an extraction solvent is adopted, large-polarity by-products can be removed to a great extent, and residues are simply stirred and washed by n-hexane, so that a fluorochloridone raw material medicine with the purity of more than 95% can be obtained.
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Paragraph 0026; 0031-0039; 0043-0049; 0053-0059; 0063-0068..
(2021/07/10)
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- Process for improving cyclization synthesis yield of fluorochloridone
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The invention relates to a process for improving a cyclization synthesis yield of fluorochloridone. The process comprises the following steps: performing a reaction by taking N-allyl-N-dichloroacetyl-meta-trifluoromethylaniline as a raw material, taking anhydrous 1,2-dichloroethane as a solvent, wherein the amount of the solvent is controlled to be 10-45mL based on each gram of the raw material, taking cuprous chloride as a main catalyst, taking 2,2'-dipyridyl as a co-catalyst, wherein the molar ratio of the main catalyst to the co-catalyst is controlled to be 1:1, the usage amount of the catalysts is 10-30mol%, and the reaction temperature is controlled to be 70-90 DEG C until the raw material disappears, filtering the reaction liquid through a silica gel column, and performing elution with dichloromethane to obtain the fluorochloridone. Compared with the prior art, the process provided by the invention only needs the short silica gel column for filtration, and can obtain the fluorochloridone original medicine with the content of 95% or more, the ratio of a trans-form medicine to a cis-form medicine of 3:1 or more and the cyclization yield of 95% or more without the need of purification such as distillation and recrystallization.
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Paragraph 0012-0018
(2018/04/21)
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- Synergistic herbicidal compositions
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Synergistic herbicidal activity is displayed by compositions comprising the following two components: (a) a pyrrolidone of the formula STR1 in which X is selected from the group consisting of hydrogen, chlorine and methyl; Y is selected from the group consisting of hydrogen, chlorine and bromine; Z is selected from the group consisting of chlorine and bromine; R1 is selected from the group consisting of hydrogen and C1 -C4 alkyl; R2 is selected from the group consisting of hydrogen, halogen, C1 -C4 alkyl, acetyl, trifluoromethyl, nitro, cyano, C1 -C4 alkoxy, C1 -C4 alkylthio, C1 -C4 alkylsulfinyl, C1 -C4 alkylsulfonyl, trifluoromethylsulfinyl, trifluoromethylsulfonyl, pentafluoropropionamido, and 3-methylureido; and R3 is selected from the group consisting of hydrogen, C1 -C4 alkyl, chlorine and trifluoromethyl; and (b) a phosphonic acid of the formula STR2 in which R4 is selected from the group consisting of C1 -C4 alkyl, C1 -C4 haloalkyl, and --CH2 NHCH2 COOH, at a weight ratio of (a) to (b) of from about 0.1:1 to about 20:1.
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- Synergistic herbicidal compositions
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Synergistic herbicidal activity is displayed by composition comprising the following two components: (a) a pyrrolidone of the formula STR1 in which X is selected from the group consisting of hydrogen, chlorine, and methyl; Y is selected from the group consisting of hydrogen, chlorine, and bromine; Z is selected from the group consisting of chlorine and bromine; R1 is selected from the group consisting of hydrogen and C1 -C4 alkyl; R2 is selected from the group consisting of hydrogen, C1 -C4 alkyl, acetyl, trifluoromethyl, nitro, cyano, C1 -C4 alkoxy, C1 -C4 alkylthio, C1 -C4 alkylsulfinyl, C1 -C4 alkylsulfonyl, trifluoromethylthio, trifluoromethylsulfinyl, trifluoromethylsulfonyl, pentafluoropropionamido, and 3-methylureido; and R3 is selected from the group consisting of hydrogen, C1 -C4 alkyl, chlorine and trifluoromethyl; and (b) a cyclohexenedione of the formula STR2 in which R4 is 1'-(2-hydroxyethylimino)ethyl or acetyl, at a weight ratio of (a) to (b) of from about 0.01:1 to about 10:1.
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- Synergistic herbicidal compositions
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Synergistic herbicidal activity is displayed by compositions comprising the following two components: (a) a pyrrolidone of the formula STR1 in which X is selected from the group consisting of hydrogen, chlorine and methyl; Y is selected from the group consisting of hydrogen, chlorine and bromine; Z is selected from the group consisting of chlorine and bromine; R1 is selected from the group consisting of hydrogen and C1 -C4 alkyl; R2 is selected from the group consisting of hydrogen, halogen, C1 -C4 alkyl, acetyl, trifluoromethyl, nitro, cyano, C1 -C4 alkoxy, C1 -C4 alkylthio, C1 -C4 alkylsulfinyl, C1 -C4 alkylsulfonyl, trifluoromethylthio, trifluoromethylsulfinyl, trifluoromethylsulfonyl, pentafluoropropionamido, and 3-methylureido; and R3 is selected from the group consisting of hydrogen, C1 -C4 alkyl, chlorine and trifluoromethyl; and (b) a m-ureidophenyl carbamate of the formula STR2 in which R4 is C1 -C4 alkyl; R5 is C1 -C4 alkyl; and R6 is selected from the group consisting of hydrogen and C1 -C4 alkyl, 1t a weight ratio of (a) to (b) of from about 0.1: to about 50:1.
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- Synergistic herbicidal compositions
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Synergistic herbicidal activity is displayed by a composition comprising the following two components: (a) a pyrrolidone of the formula STR1 in which X is selected from the group consisting of hydrogen, chlorine and methyl; Y is selected from the group consisting of hydrogen, chlorine and bromine; Z is selected from the group consisting of chlorine and bromine; R1 is selected from the group consisting of hydrogen and C1 -C4 alkyl; R2 is selected from the group consisting of hydrogen, C1 -C4 alkyl, acetyl, trifluoromethyl, nitro, cyano, C1 -C4 alkoxy, C1 -C4 alkylthio, C1 -C4 alkylsulfonyl, C1 -C4 alkylsulfinyl, trifluoromethylthio, trifluoromethylsulfinyl, trifluoromethylsulfonyl, pentafluoropropionamido, and 3-methylureido; and R3 is selected from the group consisting of hydrogen, C1 -C4 alkyl, chlorine and trifluoromethyl; and (b) a urea of the formula STR2 in which R4 is selected from the group consisting of phenyl and substituted phenyl, wherein the substituents are selected from the group consisting of p-chlorophenoxy and alkylacetamido; R5 is selected from the group consisting of hydrogen and C1 -C4 alkyl; and R6 is selected from the group consisting of C1 -C4 alkyl and C1 -C4 alkoxy; at a weight ratio of (a) to (b) of from about 0.01:1 to about 20:1.
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- Synergistic herbicidal compositions
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Synergistic herbicidal activity is displayed by a composition comprising the following two components: (a) a pyrrolidone of the formula STR1 in which X is selected from the group consisting of hydrogen, chlorine, and methyl; Y is selected from the group consisting of hydrogen, chlorine, and bromine; Z is selected from the group consisting of chlorine and bromine; R1 is selected from the group consisting of hydrogen and C1 -C4 alkyl; R2 is selected from the group consisting of hydrogen, C1 -C4 alkyl, acetyl, trifluoromethyl, nitro, cyano, C1 -C4 alkoxy, C1 -C4 alkylthio, C1 -C4 alkylsulfonyl, C1 -C4 alkylsulfinyl, trifluoromethylthio, trifluoromethylsulfinyl, trifluoromethylsulfonyl, pentafluoropropionamido, and 3-methylureido; and R3 is selected from the group consisting of hydrogen, C1 -C4 alkyl, chlorine and trifluoromethyl; and (b) 3-amino-1,2,4-triazole, at a weight ratio of (a) to (b) of from about 0.01:1 to about 20:1.
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