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

Ozone oxidation method used for preparing halogenated acetic acid and esters of halogenated acetic acid

A technology of haloacetate and haloacetate, which is applied in the field of preparation of haloacetate or haloacetate compounds, to achieve high economic benefits and ecological effects, environmentally friendly and efficient preparation, and mild reaction conditions

Active Publication Date: 2015-05-20
LIANYUNGANG JINKANG PHARMA TECH
View PDF14 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, this requires special and expensive equipment, and on the other hand, when it is necessary to protect the environment, it also requires a more complicated discharge process.

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
  • Ozone oxidation method used for preparing halogenated acetic acid and esters of halogenated acetic acid
  • Ozone oxidation method used for preparing halogenated acetic acid and esters of halogenated acetic acid
  • Ozone oxidation method used for preparing halogenated acetic acid and esters of halogenated acetic acid

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0066] A specific embodiment of the present invention, the preparation method of haloacetic acid or haloacetate comprises the steps: under normal temperature and pressure, the haloalkane I, R 5 OH and non-alcoholic organic solvent are mixed evenly, and ozone is passed through. When the reaction of the raw materials is completed, the reaction is stopped, and the reaction liquid is washed with water and an inorganic salt solution, dried, and distilled to obtain the haloacetic acid or haloacetate compound of formula II.

[0067] The inorganic salt solution described therein includes saturated sodium bicarbonate solution, saturated sodium carbonate solution, saturated potassium carbonate solution, saturated sodium bisulfite solution, and saturated saline solution.

[0068] In an embodiment of the present invention, the reaction status of the ethyl halide substrate can be tracked and analyzed through a gas chromatographic column.

[0069] In addition, the acid (such as HI, HBr or H...

Embodiment 1

[0078] The preparation of embodiment 1 methyl bromodifluoroacetate

[0079]

[0080] At normal temperature and pressure, mix difluorodichlorodibromoethane (30g, 0.1mol), methanol (32g, 1.0mol), dichloromethane (120g, 1.4mol) and add to the reactor equipped with a condenser During the process, the ozone generator was turned on, and the ozone flow rate was 6g / h. After 3 hours, the reaction liquid was washed with water, saturated sodium bisulfite, and saturated sodium bicarbonate, and 15 g of methanol was added to the organic layer, and the reaction was continued until the conversion of raw materials was completed, and then water, saturated sodium bisulfite, saturated sodium bicarbonate, and saturated Wash with brine, dry the organic layer with anhydrous magnesium sulfate to obtain the crude product of bromodifluoroacetic acid methyl ester, transfer the obtained crude product to a rectification column for distillation, collect the fraction at 94°C-96°C, and finally obtain met...

Embodiment 2

[0081] The preparation of embodiment 2 ethyl bromodifluoroacetate

[0082]

[0083] Under normal temperature and pressure, mix difluorodichlorodibromoethane (30g, 0.1mol), ethanol (37g, 0.8mol), 1,1-dichloroethane (105g, 1.0mol), and add In the reactor of the condensing tube, the ozone generator was opened, and the ozone flow rate was 8g / h. After 2.5 hours, the reaction liquid was washed with water, saturated sodium bisulfite, and saturated sodium bicarbonate, and 20 g of ethanol was added to the organic layer, and the reaction was continued until the conversion of raw materials was completed, and then water, saturated sodium bisulfite, saturated sodium bicarbonate, and saturated Wash with brine, dry the organic layer with anhydrous magnesium sulfate to obtain the crude product of ethyl bromodifluoroacetate, transfer the obtained crude product to a rectification column for distillation, collect fractions at 111°C-113°C, and finally obtain ethyl bromodifluoroacetate The e...

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 belongs to the field of chemical synthesis, and specially relates to a preparation method of halogenated acetic acid and halogenated acetic acid ester compounds. According to the preparation method, halogenated ethane (represented by formula I) is subjected to ozone oxidation, and is reacted with water or alcohol so as to obtain halogenated acetic acid or the halogenated acetic acid ester compounds (represented by formula II).

Description

technical field [0001] The invention relates to a preparation method of haloacetic acid or haloacetate compound, in particular to preparation of haloacetic acid or haloacetate through haloethane ozonation reaction. Background technique [0002] Halogenated acetic acid or halogenated acetate compounds are mainly used to synthesize intermediates of some medicines, pesticides, liquid crystals, and fuels, and have great development prospects. At present, there are hundreds of drugs synthesized with haloacetic acid or haloacetate at home and abroad, and many drugs have become the main varieties for the treatment of certain diseases, and have become a very important category of synthetic drugs, such as the cardiovascular and cerebrovascular drugs Lyno Puli, fluoroquinolone antibiotics, antidepressant fluoxetine, and antifungal fluconazole are used in pesticides to manufacture cell division inhibitors, and are used in cotton and peanut fields to kill grasses and broad-leaved weeds....

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): C07C67/39C07C69/63C07C51/34C07C53/18
Inventor 成永之王海吉利
Owner LIANYUNGANG JINKANG PHARMA TECH