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Synthetic method of hexamethylene flusulfamide

A technology of cycloheximide and a synthesis method, which is applied in the field of cycloheximide, can solve the problems of unhelpful growth of by-product crops, difficult separation and removal, expensive raw material prices, etc., and achieves clean production, cost reduction, and product quality. high purity effect

Inactive Publication Date: 2012-12-26
CHINA AGRI UNIV +1
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Problems solved by technology

The raw materials used in this invention are relatively expensive, and the by-products after the reaction are not beneficial to crop growth, and are difficult to separate and remove

Method used

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  • Synthetic method of hexamethylene flusulfamide

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Embodiment

[0029] As shown in the accompanying drawing, the specific synthesis method of cyclazone can be decomposed into the following 4 processes:

[0030] (1) Preparation of sulfur trioxide-dioxane complex (1:1)

[0031] A mixture of 127.9g (1.45 mol) 1,4-dioxane and 150 ml 1,2-dichloroethane was added dropwise to 116.3g (1.45 mol) sulfur trioxide under mechanical stirring and ice-bath cooling and 400ml of 1,2-dichloroethane solution, white solids are produced, and the temperature rises rapidly, and the temperature is controlled within 20°C. After dropping half of the dichloroethane solution of dioxane, the temperature rises slowly. At this time, speed up the dropping rate, and after the dropwise addition, continue to stir for 30 min, and the obtained sulfur trioxide complex suspension is directly used for the next reaction, or sealed and stored in a minus 25°C refrigerator for future use.

[0032] (2) Preparation of ammonium 2-oxocyclohexylsulfonate

[0033] Add 157g (1.6 mol) cycl...

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Abstract

The invention provides a synthetic method of hexamethylene flusulfamide. The synthetic method comprises the following steps: reacting to obtain 2-oxocyclohexyl ammonium sulphonate and ammonium sulfate by adopting cyclohexanone, 1, 4-dioxane, sulfur trioxide and ammonia as the raw materials; washing via reaction product through absolute methanol, and leaching to separate ammonium sulfate; and then carrying out reaction among 2-oxocyclohexyl ammonium sulphonate, oxalyl chloride and 2-trifluoromethyl-4-chloroaniline to obtain hexamethylene flusulfamide. According to the synthetic method provided by the invention, KOH solution is replaced via the ammonia, thus, the reaction endpoint is easily controlled; the byproduct ammonium sulfate can be used as chemical fertilizer after being separated, and the generation of three wastes such as waste barium sulfate can be removed; the reaction is easy to operate, the post-processing is simple to carry out, the product is high in purity and high in yield, and the method is suitable for large-scale industrial application.

Description

technical field [0001] The present invention relates to a chemical synthesis technology of the compound N-(2-trifluoromethyl-4-chlorophenyl)-2-oxocyclohexylsulfonamide (abbreviated as cyclohexasulfame in the present invention) in the field of agricultural chemistry . Background technique [0002] Cyclohexasulfame can be used as a fungicide, which can be used to prevent and control various crop diseases such as tomato gray mold, rape sclerotinia, and cucumber brown spot. The general molecular structure formula and chemical synthesis technology of its series of compounds are disclosed in the patent application number 200510085408.4 "2-oxocycloalkylsulfonamide, its preparation method and use as a fungicide". In this invention, take cyclohexanone or cycloheptanone as a raw material to synthesize the 2-oxocycloalkylsulfonic acid potassium salt intermediate first, and after the latter makes 2-oxocycloalkylsulfonyl chloride with oxalyl chloride, then combine with The substituted...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/14C07C303/38C05C3/00
Inventor 梁晓梅张建军张海滨王道全孔涵楚薛健
Owner CHINA AGRI UNIV
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