- Synthetic method of dicyclanil
-
The invention discloses a synthetic method of dicyclanil. The sodium dicyandiamide and malononitrile are used as initial raw materials, a crude dicyandiamide product is obtained through condensation,cyclization and amination reactions, and a refined dicyandiamide product is obtained through decoloration and refining. The synthetic route is short, the process is green and environment-friendly, andmethyl mercaptan is not generated; the method has the advantages of mild reaction conditions, no need of pressurized ammonification, low equipment requirements and simple operation, and is suitable for domestic industrial production. The total yield reaches 65% or above, and the product purity reaches 99% or above.
- -
-
Paragraph 0041; 0052-0056; 0060; 0065-0066; 0070; 0075-0076
(2020/05/01)
-
- Dicyclanil preparation method
-
The invention relates to the field of insecticides, in particular to a dicyclanil preparation method. The method comprises the steps as follows: 500 g of absolute methanol and 270 g of a sodium methylate methanol solution are added to a 2 L four-neck flask, the obtained solution is cooled to 0-5 DEG C in an ice-water bath, 72.8 g of malononitrile is added, stirring is performed for 30 min, the temperature is kept at 0-5 DEG C, 146.5 g of N-cyanoimido-S, S-dimethyl-dithiocarbonate is added in batches, the obtained mixture is stirred at 0-5 DEG C to react for 12 h, filtration is performed afterthe reaction, a filter cake is washed with 100 mL of cold absolute methanol, and the filter cake is drained and directly used in the next reaction without drying; the wet product is dissolved in 860 gof water, the obtained solution is added to a four-neck flask and stirred to be dissolved, the temperature is decreased to 0-5 DEG C in an ice-water bath, 1,200 g of industrial hydrochloric acid is dropwise added for about 4-5 h, the obtained mixture is stirred at 0-5 DEG C and stays overnight after addition, filtration is performed after complete reaction, a filter cake is washed with water andwashed twice with 10% sodium carbonate, the washed filter cake is dried in a drying oven after being drained, and 157 g of a dried product is obtained. The process is simple, the reaction is safe, theproduction cost is greatly reduced, and the product purity is improved.
- -
-
Paragraph 0008
(2018/04/02)
-
- A preparation method of ground past Neil
-
The invention discloses a preparation method of dicyclanil, belongs to the field of preparation of growth regulators, and solves the problem that the existing dicyclanil production process is high in synthetic condition, great in toxicity of synthetic raw materials and low in reaction yield. The preparation method comprises the following steps: carrying out substitution reaction on guanidine hydrochloride and bromocyclopropane; carrying out closed-ring reaction on the product obtained from the former step and 2-fluoropropiondiamide; and finally substituting florine on aromatic rings by providing cyan groups from potassium ferrocyanide to obtain a dicyclanil product. The preparation method disclosed by the invention is simple in operating step, low in price of materials and high in yield, and the obtained product is high in purity and shallow in color, and dicyanomethane which is relatively great in toxicity is not used in the production process.
- -
-
Paragraph 0013; 0041
(2017/04/25)
-
- Active agent combinations
-
The novel active compound combinations of extracts from seeds of the neem tree and the active compounds of groups (B) to (F) listed in the description have very good insecticidal and acaricidal properties.
- -
-
-