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

Preparation method of substituted sulfinate

A technology of sulfinate and sulfonyl chloride, which is applied in the field of preparation of sulfinate and its derivatives, can solve the problems of complex experimental operation, high reaction cost, harsh reaction conditions, etc., and achieve simple process and high product purity Effect

Pending Publication Date: 2020-12-18
JIANGSU YANGNONG CHEM +1
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the currently reported synthetic methods for sulfinic acid have more or less disadvantages, such as the need to use expensive transition metal catalysts and ligands, the reaction substrate needs to have specific functional groups, the reaction conditions are harsh, and the reaction time Long, complicated experimental operation, high reaction cost, etc.

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 of substituted sulfinate
  • Preparation method of substituted sulfinate
  • Preparation method of substituted sulfinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation method of substituted sulfinic acid salt, take benzenesulfinyl chloride hydrolysis reduction to obtain benzenesulfinic acid sodium salt as example:

[0025] Add 20.1g (0.402mol) of hydrazine hydrate to 300g of water, add 40.8g (0.385mol) of sodium carbonate, and then heat up to dissolve. At 60°C, add 111g (0.629mol) of benzenesulfonyl chloride dropwise, and keep it warm for 2 hours to synthesize the solution. The sodium salt of benzenesulfinic acid was obtained by cooling and filtering, and the purity analysis was performed by HPLC. The results are summarized in Table 1.

Embodiment 2-7

[0027] The operation process of embodiment 2-7 is identical with embodiment 1, and the sulfonyl chloride that raw material replaces is as shown in table 1, and hydrolysis temperature is as shown in table 1, obtains corresponding sulfinic acid salt, HPLC carries out purity analysis, and the result is summarized in table 1 in:

[0028] Table 1: Comparative Examples of Reductive Hydrolysis of Substituted Sulfonyl Chlorides

[0029]

Embodiment 8

[0031] Add 40.3g (0.63mol) of methylhydrazine hydrate to 300g of water, add 40.8g (0.385mol) of sodium carbonate, and then heat up to dissolve. At 60°C, add 111g (0.629mol) of benzenesulfonyl chloride dropwise, and keep warm for 2.5h , the synthetic solution was cooled and filtered to obtain sodium benzenesulfinate, and HPLC carried out the purity analysis, and the sulfinate accounted for 95.2% in the mixture, and the product sodium phenylsulfinate with a content of 98.1% was obtained after post-treatment, and the yield (with Benzenesulfonyl chloride) 92.2%

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 discloses a preparation method of substituted sulfinate, which comprises the following steps: by using substituted sulfonyl chloride as a raw material, carrying out hydrolysis reductionreaction on the substituted sulfonyl chloride in water in the presence of a reducing agent and an acid-binding agent to generate the corresponding substituted sulfinate. The method is a novel method which is easy to implement and suitable for industrial scale production and is used for preparing sulfinate and derivatives thereof. The method is simple in technological process, high in product purity and safe and environment-friendly, wherein the waste gas, solid and liquid are easy to treat.

Description

technical field [0001] The invention relates to a new preparation method of sulfinic acid salt and its derivatives, which can be obtained in the form of sodium salt and further reacted to generate analogues, belonging to the technical field of organic synthesis. Background technique [0002] Sulfinic acid and its salts are widely used in the fields of medicine, printing and dyeing, pesticides, etc. They can not only be used as coupling reagents to prepare various isomeric and heterocyclic The reaction is an important intermediate for the preparation of sulfone, sulfoxide, sulfonamide, sulfonyl chloride and other organic compounds containing sulfonyl (-SO_2-). In recent years, coupling reactions based on the participation of sulfinic acid and its salts have developed rapidly, and chemical bonds such as carbon-carbon bonds, carbon-heterobonds, and sulfur-heterobonds can be constructed under different reaction conditions, thereby preparing various types of Organic compounds wi...

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): C07C313/04C07D213/71C07C315/00C07C317/14
CPCC07C313/04C07D213/71C07C315/00
Inventor 吴孝举姜友法王宝林冯广军孙迎东程炎
Owner JIANGSU YANGNONG CHEM