Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of improved preparation method of spiroxamine ethanolamine salt

A technology for spirozide ethanolamine salt and spirozide, which is applied in the field of improved preparation of spirozide ethanolamine salt, can solve problems such as energy consumption and loss, increase in safety hazards, etc., to increase safety, improve killing effect, The effect of excellent suspension rate

Active Publication Date: 2018-10-12
苏州市罗森助剂有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of a large amount of solvent in this process, potential safety hazards increase, the safety level of the workshop is improved, and there is energy consumption and loss during solvent recovery

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The present embodiment provides a kind of improved preparation method of spiroxamine ethanolamine salt, it comprises the following steps:

[0014] (a) Into a 1000ml four-neck flask, add 60g of spiroxamine (dry weight), 500ml of water and 0.01g of MF (sodium methylenebismethyl naphthalene sulfonate) successively, stir and raise the temperature to 80°C, and keep it warm for 1 hour;

[0015] (b) Under the condition of stirring, add 20g of monoethanolamine dropwise to the four-necked flask (the dropping time is controlled at about 30 minutes), after the dropwise addition is completed, keep the temperature at 80°C for 4 hours, filter with suction and wash with water until the filtrate is clear , dry it; the measured chromatographic content is (mass concentration measured by liquid chromatography) 98.2%; then the obtained spiroxamin ethanolamine salt is made into a wettable powder, and the suspension rate is measured to be 94%.

Embodiment 2

[0017] The present embodiment provides a kind of improved preparation method of spiroxamine ethanolamine salt, it comprises the following steps:

[0018] (a) Into a 1000ml four-necked flask, add 60g of spiroxamine (dry weight), 360ml of water and 0.06g of MF (sodium methylenebismethyl naphthalene sulfonate) successively, stir and raise the temperature to 80°C, and keep it warm for 1 hour;

[0019] (b) Under the condition of stirring, add 20g of monoethanolamine dropwise to the four-necked flask (the dropping time is controlled at about 30 minutes), after the dropwise addition is completed, keep the temperature at 80°C for 4 hours, filter with suction and wash with water until the filtrate is clear , dry it; the measured chromatographic content is (mass concentration measured by liquid chromatography) 97.6%; then the obtained spiroxamin ethanolamine salt is made into a wettable powder, and the suspension rate is measured to be 93%.

Embodiment 3

[0021] The present embodiment provides a kind of improved preparation method of spiroxamine ethanolamine salt, it comprises the following steps:

[0022] (a) Into a 1000ml four-neck flask, add 60g of spiroxamine (dry weight), 900ml of water and 0.24g of MF (sodium methylenebismethyl naphthalene sulfonate) successively, stir and raise the temperature to 80°C, and keep it warm for 1 hour;

[0023] (b) Under the condition of stirring, add 20g of monoethanolamine dropwise to the four-necked flask (the dropping time is controlled at about 30 minutes), after the dropwise addition is completed, keep the temperature at 80°C for 4 hours, filter with suction and wash with water until the filtrate is clear , dry it; the measured chromatographic content is (mass concentration measured by liquid chromatography) 97.5%; then the prepared spiroxamin ethanolamine salt is made into a wettable powder, and the suspension rate is measured to be 92%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to an improved preparation method for niclosamide ethanolamine. The method includes the following steps: (a) successively adding niclosamide, water and an additive into a reaction container, stirring the components and increasing the temperature to 60-90 DEG C, and maintaining the temperature for 0.5-2 h; (b) under stirring, dropwisely adding monoethanolamine into the reaction container, and then performing a temperature maintained reaction at 60-80 DEG C for 2-5 h, performing suction filtration, washing a product with water until a filtrate is clear, and drying the product. In the method, the niclosamide is dispersed in water by means of the additive, so that a reaction to the niclosamide and the monoethanolamine is carried out at a certain temperature. The method avoids usage of an organic solvent and is more environment-friendly, and improves production safety. The niclosamide ethanolamine has high suspension rate and is improved in killing effect on aquatic animals, such as ampullaria gigas.

Description

technical field [0001] The invention belongs to the field of chemical auxiliaries, and in particular relates to an improved preparation method of sppiroxamin ethanolamine salt. Background technique [0002] Ethanolamine salt of spiroxamin is a drug widely used to kill snails. The current production method is to make a slurry of spiroxamine with a large amount of ethanol or methanol to form a suspension, and then raise the temperature to slightly lower than that of the corresponding alcohol. Slowly add a certain amount of monoethanolamine at the boiling point to make it react to generate spiroxamine ethanolamine salt; then filter, the filtrate is rectified in a rectification tower, the solvent is recovered, and the filter cake is washed with water to obtain the product spiroxamine ethanolamine salt . Due to the use of a large amount of solvent in this process, potential safety hazards increase, the safety level of the workshop is improved, and energy consumption and loss occ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/14C07C235/64C07C213/00C07C215/08
CPCC07C213/00C07C231/14C07C235/64C07C215/08
Inventor 徐新连
Owner 苏州市罗森助剂有限公司