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Process for producing 2-amino-4-dimethylin-6-trifluoro oxethyl-1,3,5-triazine

A technology of trifluoroethoxy and dimethylamine, which is applied in the field of preparation of pesticide intermediates, can solve the problems of increased production cost, cumbersome process, hidden danger of production safety, etc., and achieves reduction of production cost, simple process and reduced production cost effect

Active Publication Date: 2011-05-11
JIANGSU INST OF ECOMONES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method mainly has following deficiency: (1) product yield is on the low side, and three-step total yield only has 56%, thereby makes its production cost too high, does not reach industrialized production requirement
(2) Ammonia gas is used in production, which is difficult to measure accurately, which affects the purity of intermediate products
(3) The process operation is complicated, and the intermediates in each step need to be separated and filtered, and the product in the second step needs to be recrystallized. The process is extremely cumbersome, which brings difficulties to its industrial production
(4) The third step uses sodium metal to bring hidden dangers to production safety
(5) The trifluoroethanol in this method is used both as a reactant and as a solvent, and the price of trifluoroethanol is relatively high (60,000 yuan / ton), which greatly increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] ①Add 50g of cyanuric chloride (0.27mol) and 200ml of acetone into a reaction flask equipped with a stirrer, a thermometer and a dropping funnel, and cool to 3°C with an ice bath while stirring. Add 34g of ammonia solution (0.54mol) with a concentration of 27wt% dropwise into the solution, heat up to 20°C and stir the reaction for 2h after dropping, to obtain 2-amino-4,6-dichloro-1,3,5-triazine solution .

[0010] ② Cool the 2-amino-4,6-dichloro-1,3,5-triazine solution to 7° C. in an ice bath, and add 73.8 g of a 33 wt% dimethylamine aqueous solution (0.54 mol) dropwise to the solution . After dropping, the temperature was raised to 20°C and the reaction was stirred for 2h. Filter and wash with water to obtain 2-amino-4-dimethylamino-6-chloro-1,3,5-triazine with a purity of 98.3%.

[0011] ③ Add 27g of trifluoroethanol (0.27mol), 200ml of acetone and 21.6g of 50wt% sodium hydroxide aqueous solution (0.27mol) in a reaction flask equipped with a stirrer, a thermometer a...

Embodiment 2~ Embodiment 6

[0013] Each embodiment is basically the same as Embodiment 1, and the differences are shown in Table 1.

[0014] Table 1

[0015]

[0016] 2-amino-4-dimethylamino

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PUM

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Abstract

The invention discloses a method for preparing 2-amido-4-dimethylamino-6-trifluoro oxyethyl group-1, 3, 5-triazine. The method comprises the following steps: (1) cyanuric chloride and acetone are mixed, are subjected to ice-bath to be cooled to a temperature between 0 and 10 DEG C, are dripped with hartshorn, and be heated up to a temperature to between 15 and 25 DEG C, and stirred and react for one to three hours; (2) the solution is subjected to ice-bath to be cooled to a temperature between 0 and 10 DEG C, is dripped with dimethylamine agueous solution, is stirred and react for one to three hours, and is filtered and washed to obtain 2-amido-4-dimethylamino-6-chloro-1, 3, 5-triazine; and (3) the 2-amido-4-dimethylamino-6-chloro-1, 3, 5-triazine obtained from the step (2) is added to trifluoro sodium alcoholate organic solution, is subjected to reflux reaction for two to six hours, and is subjected to post treatment to obtain the 2-amido-4-dimethylamino-6-chloro-1, 3, 5-triazine. The preparation method has the advantages of simple operation, no separation of intermediate products, high product yield, high purity and easy industrialized production.

Description

technical field [0001] The invention relates to a preparation method of a pesticide intermediate, in particular to a preparation method of 2-amino-4-dimethylamino-6-trifluoroethoxy-1,3,5-triazine. Background technique [0002] Flusulfasulfuron-methyl is a post-emergence herbicide with high safety in sugar beet fields. It can control many broad-leaved weeds and grass weeds. 2-Amino-4-dimethylamino-6-trifluoroethoxy-1 , 3,5-triazine is the key intermediate in the synthesis of flusulfuron-methyl. [0003] Chinese patent literature CN1778798A discloses a preparation method of 2-amino-4-dimethylamino-6-trifluoroethoxy-1,3,5-triazine, which uses cyanuric chloride as raw material, In the presence of acetone solvent, ammonia gas is passed through, the product is reacted with dimethylamine, and the intermediate product obtained is reacted with sodium trifluoroethoxide to obtain 2-amino-4-dimethylamino-6-trifluoroethane Oxy-1,3,5-triazine. This method mainly has the following defic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/52
Inventor 孔繁蕾孙永辉史志兵
Owner JIANGSU INST OF ECOMONES
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