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Preparation method for intermediate epichlorophdrin of herbicide pretilachlor

A technology of pretilachlor and trichlorether, which is applied in the field of compound preparation, achieves good industrialization implementation value and social and economic benefits, mild reaction conditions, and safe and reliable operation process

Inactive Publication Date: 2011-08-17
HANGZHOU VOCATIONAL & TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Method ①Although the yield is high, a large amount of sulfur dioxide tail gas is released during the reaction process, and DMF is difficult to recover, resulting in a large amount of waste gas and wastewater, and the treatment cost is high; Method ②The yield is low, and ethylene glycol monopropyl ether is under strong acidic conditions Unstable, in addition, the source of dry hydrogen chloride is difficult, and there are safety hazards in the use process
Method ③ The obtained product contains a large amount of by-product phosphoric acid, and phosphorus oxychloride is used as a chlorinated reagent to seriously corrode the equipment, and a large amount of phosphorus-containing wastewater is difficult to treat, and the pollution problem is serious
Above-mentioned several methods are all not suitable for industrialized production of chlorether because there are different defectives

Method used

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Examples

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Effect test

Embodiment 1

[0012] Example 2

[0013] The preparation method of the herbicide pretilachlor intermediate chloroether described in this embodiment, the amount of its described feeding material ratio ethylene glycol monopropyl ether: bis (trichloromethyl) carbonate: catalyst is 1: 0.4 : 0.2, the charging amount of ethylene glycol monopropyl ether is 10.5g (0.1mol), the charging amount of bis(trichloromethyl) carbonate is 12g (0.04mol), the catalyst is pyridine, and the consumption is 1.6g (0.02mol) , the organic solvent is toluene, and the consumption is 40ml, which is 3.3 times of the quality of ethylene glycol monopropyl ether.

[0014] Reaction temperature is 100~110 ℃, other operation is the same as embodiment 1, obtains product 10.8g, product yield 88.5%, purity (GC) 98.5%, boiling point 130~132 ℃.

Embodiment 2

[0016] The preparation method of the herbicide pretilachlor intermediate chlorether described in this embodiment, the amount of its described feeding material ratio ethylene glycol monopropyl ether: bis (trichloromethyl) carbonate: catalyst is 1: 0.35 : 0.1, the intake of ethylene glycol monopropyl ether is 10.5g (0.1mol), the intake of bis(trichloromethyl)carbonate is 10.5g (0.035mol), the catalyst is triethylamine, and the consumption is 1g (0.01 mol), the organic solvent is ethylene dichloride, and the consumption is 35ml, which is 4.2 times of the quality of ethylene glycol monopropyl ether.

[0017] Reaction temperature is 70~80 ℃, other operation is the same as embodiment 1, obtains product 10.5g, product yield 86%, purity (GC) 98.9%, boiling point 128~131 ℃.

Embodiment 3

[0019] The preparation method of the herbicide pretilachlor intermediate chloroether described in this embodiment, the amount of its described feeding material ratio ethylene glycol monopropyl ether: bis (trichloromethyl) carbonate: catalyst is 1: 0.4 : 0.2, the charging amount of ethylene glycol monopropyl ether is 10.5g (0.1mol), the charging amount of bis(trichloromethyl) carbonate is 12g (0.04mol), the catalyst is triethylamine, and the consumption is 2g (0.02mol ), the organic solvent is chlorobenzene, and the consumption is 40ml, which is 4.2 times of ethylene glycol monopropyl ether quality.

[0020] Reaction temperature is 120~130 ℃, other operation is the same as embodiment 1, obtains product 10.7g, product yield 87.5%, purity (GC) 99.2%, boiling point 130~131 ℃.

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Abstract

The invention relates to a method for preparing a herbicide pretilachlor intermediate chloride ether, which comprises: under the action of an organic amine catalyst, the chloride ether can be obtained by reacting ethylene glycol monopropyl ether with bis (trichloromethyl) hydroxyphenyl in the organic solvent according to the following chemical equation: HOC2H4OC3H7+Cl3COCOOCCl3 - ClC2H4OC3H7+CO2+HCl. The method substitutes bis(trichloromethyl) hydroxyphenyl for traditional chlorination reagents, such as thionly chloride, phosphorus oxychloride and hydrogen chloride, etc., and the potential safety hazard can be eliminated from the process source by using the novel chlorination reagent. Simultaneously, the emissions of pollutants are greatly reduced; the method is a cleaning process with mild reaction conditions, safe and reliable operating process and high product yield, and has good industrialization implementation value and social economic benefits.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of a herbicide pretilachlor intermediate chlorether. Background technique [0002] Chloroethyl propyl ether (2-n-propoxychloroethane), referred to as chloroether, is an important intermediate for the synthesis of the herbicide pretilachlor, which is a high-efficiency, low-toxicity, early-stage broad-spectrum rice field special choice The herbicide at bud stage was successfully developed by Ciba-Geigy in Switzerland. It is widely used and highly appraised by the agricultural plant protection department. As an important intermediate of chloroethers, how to adopt a clean and efficient preparation method has attracted great attention. At present, the preparation methods of chloroethers mainly include: ① in the presence of a large amount of acid-binding agent DMF, chlorination with thionyl chloride, the yield is about 90%, ② in the presence of anhydrous zinc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/22C07C43/12
Inventor 童国通谢建武毛伟春
Owner HANGZHOU VOCATIONAL & TECHN COLLEGE
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