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Process for producing bactericide of flutriafol midbody

A technology for triazole alcohol and intermediates, applied in the field of preparation of intermediates, can solve the problems of low intermediate yield, large steric hindrance, difficulty in achieving quality and yield, etc., and achieves simple process, control of impurity content, The effect of improving purity

Active Publication Date: 2009-05-13
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The weak point of said method is: the preparation of above-mentioned Grignard reagent is more difficult, is difficult to reach desirable quality and yield, simultaneously in the Grignard reaction that generates triadol intermediate, due to the steric position of Grignard reagent and ketone The resistance ratio is relatively large, resulting in a relatively low yield of intermediates

Method used

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  • Process for producing bactericide of flutriafol midbody
  • Process for producing bactericide of flutriafol midbody
  • Process for producing bactericide of flutriafol midbody

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of 2,4-difluorobenzophenone

[0030] 104g (99%, 1.08mol) fluorobenzene, 152g (99%, 1.14mol) AlCl 3 Put into 300g of nitrobenzene respectively, add 150g (99%, 0.95mol) o-fluorobenzoyl chloride dropwise, react at 20-50°C for 4h, after the reaction is completed, add water to separate layers, then wash with alkaline water until neutral, and depressurize The solvent was removed to obtain 190 g of 2,4-difluorobenzophenone with a content of 99%.

[0031] (2) Preparation of onium salt

[0032] 65g (99%, 1.05mol) of anhydrous dimethyl sulfide, 78g (99%, 1mol) of dimethyl sulfoxide, were respectively dropped into a 2L reaction flask equipped with a condenser tube, and 126g (99 %, 1mol) dimethyl sulfate, stirred for 4 hours, and then stood at room temperature overnight, and the obtained onium salt was directly used for the next reaction.

[0033] (3) Preparation of Triconazole Intermediate

[0034] In the above-mentioned reaction solution, add 600g toluene, the...

Embodiment 2

[0036] (1) Preparation of 2,4-difluorobenzophenone

[0037] 104g (99%, 1.08mol) fluorobenzene, 152g (99%, 1.14mol) AlCl 3 Put into 300g of fluorobenzene respectively, add 150g (99%, 0.95mol) o-fluorobenzoyl chloride dropwise, react at 20-50°C for 4h, after the reaction is completed, add water to separate layers, add alkaline water to wash until neutral, decompress to remove The solvent was removed to obtain 190 g of 2,4-difluorobenzophenone with a content of 99%.

[0038] (2) Preparation of onium salt

[0039] 65g (99%, 1.05mol) of anhydrous dimethyl sulfide, 50g (99%, 0.68mol) of tert-butanol are respectively dropped into a 2L reaction flask equipped with a condenser tube, and 126g (99 %, 1mol) dimethyl sulfate, stirred for 4 hours, and then stood at room temperature overnight, and the obtained onium salt was directly used for the next reaction.

[0040] (3) Preparation of Triconazole Intermediate

[0041] In above-mentioned reaction solution, add 600g pure benzene, then ...

Embodiment 3

[0043] (1) Preparation of 2,4-difluorobenzophenone

[0044] 104g (99%, 1.08mol) fluorobenzene, 152g (99%, 1.14mol) AlCl 3 Put into 300g of dichloroethane respectively, add dropwise 150g (99%, 0.95mol) o-fluorobenzoyl chloride, react at 20-50°C for 4h, after the reaction is completed, add water to separate layers, then add alkaline water to wash until neutral, reduce The solvent was removed by pressure to obtain 190 g of 2,4-difluorobenzophenone with a content of 99%.

[0045] (2) Preparation of onium salt

[0046] 65g (99%, 1.05mol) of anhydrous dimethyl sulfide, 60g (99%, 0.71mol) of dichloromethane were dropped into a 2L reaction flask equipped with a condenser tube respectively, and 126g (99 %, 1mol) dimethyl sulfate, stirred for 4 hours, and then stood at room temperature overnight, and the obtained onium salt was directly used for the next reaction.

[0047] (3) Preparation of Triconazole Intermediate

[0048]To the above reaction solution, add 600g of dichloromethane...

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Abstract

The invention discloses a method for preparing an intermediate of flutriafol bactericide, which comprises the following three steps: a first step, that is, dimethyl sulphide and dimethyl sulfate react in organic solvent to generate onium salt; a second step, that is, fluorobenzene and o-fluorobenzene formyl chloride are subjected to Friedel-Crafts reaction to generate 2, 4-difluoro diphenyl ketone; and a third step, that is, the 2, 4-difluoro diphenyl ketone and the onium salt react under alkaline condition to obtain the intermediate of flutriafol with high content. The method effectively controls the content of impurities in the intermediate of the flutriafol below 0.5 percent.

Description

technical field [0001] The invention relates to a preparation method of the agricultural fungicide triconazole, in particular to a preparation method of an intermediate required for the preparation of triconazole. Background technique [0002] Triazole is the abbreviation of 1-(2-fluorophenyl)-1-(4-fluorophenyl)-1-hydrogen-1,2,4-triazole-1-ethanol, which is a protective and therapeutic The active systemic triazole fungicides can be absorbed by roots, stems, and leaves, and can quickly conduct upwards in the plant to prevent and control diseases caused by ascomycetes, basidiomycetes, and half-knowledge fungi, especially for wheat Take-all, powdery mildew, rust, root rot, rice bad fungus, and banana leaf spot have good control effects. [0003] The preparation of Fenconazole laboratory adopts the reaction of o-fluorobromobenzene and metal magnesium in ether solvent to generate Grignard reagent, and the Fried-Crafts acylation reaction of fluorobenzene and chloroacetyl chloride...

Claims

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Application Information

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IPC IPC(8): C07D303/08C07D301/02
Inventor 余志强周耀德余强
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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