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

Preparation method for 1-methylamino-1-methylthio-2-nitroethylene

A technology based on nitroethylene and methylthio, which is applied in the preparation of sulfides and organic chemistry, and can solve problems such as emission restrictions, damage to the health of operators, and foul odors in the final product.

Inactive Publication Date: 2014-10-29
石家庄康坦福化工科技有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Today, the generation of methyl mercaptan has introduced environmental issues and its discharge is restricted
In the process of preparing side three, once methyl mercaptan is produced, it is difficult to remove it through refining methods, resulting in a strong stench in the final product side three, which directly affects the quality of the final product and damages the health of operators

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method for 1-methylamino-1-methylthio-2-nitroethylene
  • Preparation method for 1-methylamino-1-methylthio-2-nitroethylene
  • Preparation method for 1-methylamino-1-methylthio-2-nitroethylene

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0042] The invention provides a preparation method of 1-methylamino-1-methylthio-2-nitroethylene, comprising the following steps:

[0043] Step 1: in the presence of a solvent, nitromethane, carbon disulfide and potassium hydroxide are subjected to condensation reaction to obtain the compound shown in formula II;

[0044] Step 2: taking the compound shown in formula II and methylamine through amination reaction to obtain the compound shown in formula III and sulfide ion, and the sulfide ion reacts with acid to generate hydrogen sulfide;

[0045] Step 3: take the compound shown in formula III, methylating reagent and base through methylation reaction to obtain the crude product of 1-methylamino-1-methylthio-2-nitroethylene, which is refined to obtain the compound of formula I The 1-methylamino-1-methylthio-2-nitroethylene shown;

[0046]

[0047] In some embodiments provided by the present invention, the mass ratio of nitromethane, carbon disulfide and potassium hydroxi...

Embodiment 11

[0070] The preparation of embodiment 11-methylamino-1-methylthio-2-nitroethylene

[0071] Add 100g of nitromethane, 100g of carbon disulfide, and 50mL of ethanol to a 1L reaction flask, heat to 20°C, dissolve 200g of potassium hydroxide in 300mL of ethanol, and after reflux occurs in the reaction flask, start to drop potassium hydroxide for condensation reaction , added dropwise for 1h, continued to react for 0.5h after adding potassium hydroxide dropwise, cooled to 15°C, and stirred for 0.5h to obtain 1,1-potassium disulfide-2-nitroethylene.

[0072] Dissolve 1,1-potassium disulfide-2-nitroethylene in 250mL of water, heat to 20°C, and drop 40% aqueous methylamine under the liquid to carry out amination reaction, wherein, 1,1-potassium disulfide-2 - The mass ratio of nitroethylene to methylamine is 6.25︰1, the time for dropping is 1 hour, and after the dropping, keep warm for 1 hour. After the heat preservation, cool down to 10°C, add 50 g of dilute sulfuric acid with a concen...

Embodiment 21

[0078] Preparation of Example 21-methylamino-1-methylthio-2-nitroethylene

[0079] Add 100g of nitromethane, 200g of carbon disulfide, and 100mL of methanol into a 1L reaction flask, heat to 30°C, dissolve 450g of potassium hydroxide in 600mL of methanol, and after reflux occurs in the reaction flask, start adding potassium hydroxide dropwise for condensation reaction , added dropwise for 2h, continued to react for 1h after adding potassium hydroxide dropwise, cooled to 10°C, and stirred for 0.5h to obtain 1,1-potassium disulfide-2-nitroethylene.

[0080] Dissolve 1,1-potassium disulfide-2-nitroethylene in 300mL of water, heat to 30°C, and drop 40% aqueous methylamine under the liquid to carry out amination reaction, wherein, 1,1-potassium disulfide-2 -The mass ratio of nitroethylene to methylamine is 7:1, the time for dropping is 2h, after the dropwise addition, keep warm for 1h, after the warming, cool down to 15°C, add 80g of dilute hydrochloric acid with a concentration of...

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 the field of chemical synthesis, and especially relates to a preparation method for 1-methylamino-1-methylthio-2-nitroethylene. The preparation method comprises: in the presence of a solvent, taking nitromethane, carbon disulfide and potassium hydroxide to perform a condensation reaction, so as to obtain a compound of a formula II; taking the compound of the formula II and methylamine to perform amination reaction, so as to obtain a compound of a formula III and hydrosulfide ion which is reacted with an acid for generating hydrogen sulfide; taking the compound of the formula III, a methylation reagent and an alkali to perform a methylation reaction, so as to obtain 1-methylamino-1-methylthio-2-nitroethylene crude product; and refining the crude product, so as to obtain 1-methylamino-1-methylthio-2-nitroethylene. The provided preparation method for 1-methylamino-1-methylthio-2-nitroethylene eliminates generation of a main gas pollution source methyl mercaptan, guarantees product quality, substantially reduces usage amount of the raw materials, shortens the reaction time and improves the product yield.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of 1-methylamino-1-methylthio-2-nitroethylene. Background technique [0002] Gastric ulcer refers to the tissue damage beyond the muscularis mucosa caused by the gastric mucosa being digested by the gastric digestive juice itself. It is one of the most common diseases in digestive system diseases. Its pain has the characteristics of long-term, periodic and rhythmic, and it mostly occurs in elderly male patients. Its onset is related to seasonal changes, smoking, irregular life and diet, and mental and psychological factors. In terms of pathogenesis, the occurrence of gastric ulcer is mainly related to the imbalance between the damage factors of gastroduodenal mucosa and the self-defense repair factors of the mucosa. Common causes of ulcers include Helicobacter pylori (H. pylori) infection, non-steroidal Anti-inflammatory drugs (NSAIDs, such as aspirin), abn...

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
IPC IPC(8): C07C323/27C07C319/14
Inventor 郭铭王俊起郭秀彬
Owner 石家庄康坦福化工科技有限公司