Check patentability & draft patents in minutes with Patsnap Eureka AI!

Preparation method of sodium thioacetate and method for preparing thiolactone by using sodium thioacetate

A technology of sodium thioacetate and thioacetic acid is applied in the field of the preparation of sodium thioacetate and the preparation of thiolactone by sodium thioacetate, which can solve the problems of complicated process, low yield of thioacetate, and difficulty in dehydration thoroughly. , to achieve the effect of simple method, less side reaction and guaranteed stability

Pending Publication Date: 2020-11-20
江西天新药业股份有限公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adopts the operation of on-site dehydration, the process is complicated, and the dehydration is difficult to carry out thoroughly, and the residual moisture and thioacetic acid will affect the thiolation reaction, resulting in low yield of thiolation reaction

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 sodium thioacetate and method for preparing thiolactone by using sodium thioacetate
  • Preparation method of sodium thioacetate and method for preparing thiolactone by using sodium thioacetate

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1-4

[0049] Preparation Example 1-4 is used to prepare sodium thioacetate

preparation Embodiment 1

[0051] Put 300g of anhydrous methanol and 30g of thioacetic acid into a dry three-necked flask, cool to -5°C under the protection of nitrogen, start to slowly and continuously add 23g of solid sodium methylate, control the feeding time for 1.5h, after the addition is complete, heat up to 25°C and stir for 3h . The heat preservation reaction at 25°C was completed, and the methanol was recovered under reduced pressure under 60°C until the solid precipitated, cooled to 0°C and filtered, the filter cake was washed with 30mL of methanol, and dried to obtain 35.7g of solid, with a yield of 91.3% (content: 99.1% by weight, Loss on drying: 0.2% by weight).

[0052] The sodium thioacetate obtained is characterized: (1) pH value is 8; (2) content of sodium thioacetate in the dried solid of gained: it is 99.1% by weight by carrying out titration detection to sulfur in sodium thioacetate; ( 3) Infrared spectrum (potassium bromide tablet, cm -1 ): 3421.1, 1636.3, 1563.1, 1416.3, 1350.4, ...

preparation Embodiment 2

[0054] Put 300g of anhydrous methanol into a dry three-necked flask, cool to 0°C under the protection of nitrogen, start to slowly add 30g of thioacetic acid and 77g of methanol solution of 30% sodium methoxide dropwise at the same time, control the dropping time for 1.5h, and complete the addition , heated to 25°C and stirred for 3h. The heat preservation reaction at 25°C was completed, and the methanol was recovered under reduced pressure under 60°C until the solid precipitated, cooled to 0°C and filtered, the filter cake was washed with 30mL of methanol, and dried to obtain 35.8g of solid, with a yield of 91.8% (content: 99.2% by weight, Loss on drying: 0.17% by weight).

[0055] The sodium thioacetate obtained is characterized: (1) pH value is 8; (2) content of sodium thioacetate in the dried solid of gained: it is 99.2% by weight by carrying out titration detection to sulfur in sodium thioacetate; ( 3) Infrared spectrum (potassium bromide tablet, cm -1 ): 3421.1, 1636.3...

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

PropertyMeasurementUnit
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to the field of organic chemistry, and discloses a preparation method of sodium thioacetate and a method for preparing thiolactone from sodium thioacetate, which are characterized in that the method comprises the following steps: in the presence of a first solvent, reacting RONa with thioacetic acid; wherein R is an alkyl group of C1 to C4, preferably an alkyl group of C1 toC2. The method has the advantages of simple process, cheap and easily available raw materials and high product yield, and provides convenience for industrial production of sodium thioacetate. The thiolactone prepared from the sodium thioacetate prepared by the method has the advantages of high reaction yield, few side reactions and high product purity.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of sodium thioacetate and a method for preparing thiolactone with sodium thioacetate. Background technique [0002] Thiolactone is a key intermediate in the production of biotin. It has been mostly prepared by thiolation of potassium thioacetate and chiral lactone. However, the preparation process of potassium thioacetate is complicated, resulting in high price of potassium thioacetate. And quality is difficult to control, and potassium thioacetate is unstable to water, can affect the yield of thiolation. [0003] CN103554129A discloses a preparation method of biotin intermediate thione, using a mixed solution of potassium thioacetate and thioacetic acid as a thio reagent, and (3aS, 6aR)-1,3-dibenzyl-tetrahydro- 4H-furo[3,4-d]imidazole-2,4(1H)-dione is mixed, benzene is recovered from the mixed system, after dehydration, under the protection of nitrogen, sul...

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 Applications(China)
IPC IPC(8): C07C327/06C07D495/04
CPCC07C327/06C07D495/04
Inventor 陆威汪康敏徐杰锋胡文荣司玉贵邱勤勇郭军
Owner 江西天新药业股份有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com