Industrial preparation method of heterocyclic derivative
A derivative and industrial technology, applied in the field of industrial preparation of heterocyclic derivatives, can solve the problems of lengthy synthetic routes, lower production efficiency, and higher production costs, and achieve the effects of increased operational difficulties, increased costs, and convenient post-processing
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0058] Example one
[0059]
[0060] 700g of furan (dissolved to 1000ml of tetrahydrofuran) is slowly added dropwise to 230g of sodium metal sand (an electron transfer aid can be added during the reaction, such as α-methylstyrene, etc.), and react at room temperature for 2-4 hours. Add 1500g diethyl oxalate dropwise while stirring, react at room temperature for 2 hours, filter, and neutralize the reaction solution to pH=6.5-7.5, extract twice with 500ml ethyl acetate, take the organic layer, distill off the solvent to obtain 1519g product, the product After reduction, the final ester compound can be obtained.
Example Embodiment
[0061] Example two
[0062]
[0063] Slowly add 900 g of p-picoline to 400 g of potassium metal, and react under reflux for 1 hour. After cooling to room temperature, add 1400 g of diethyl oxalate dropwise while stirring, and react under reflux for 4 hours, and then hot filter to neutralize the reaction solution to pH =6.5-7.5, extract twice with 500ml ethyl acetate, take the organic layer, evaporate the solvent to obtain 1732g product.
[0064] In this reaction, it can also be considered to protect the N on the pyridine ring before proceeding.
Example Embodiment
[0065] Example three
[0066]
[0067] 900g 2-methylfuran was slowly added dropwise to 1500g tert-butyllithium, and reacted under reflux for 4 hours. After cooling to room temperature, 1460g diethyl oxalate was added dropwise while stirring, and reacted under reflux for 1 hour. 1701g of product was obtained by distillation .
PUM
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.
© 2023 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap