Modified synthetic method of dicyclopropyl ketone
A technology of dicyclopropyl ketone and synthesis method, which is applied in the field of improved preparation, can solve the problems of prone to material flushing accidents, unstable yield, poor controllability, etc., and achieve the reduction of water-soluble impurities, high product yield, and environmental protection The effect of pressure reduction
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0037] Example 1
[0038] In a 1000mL four-necked flask, equipped with a thermometer, electric stirrer, reflux condenser, U-shaped calcium chloride drying tube. Under stirring, 60 g of toluene and 48.8 g of solid sodium methoxide were added, heated to increase the internal temperature to 75°C, and 137.6 g of γ-butyrolactone was added dropwise. After the dripping is completed, the temperature is raised to the internal temperature of 80-90°C to react for more than 2 hours. Then, the temperature was lowered to room temperature, 402g of pre-frozen concentrated hydrochloric acid was added, and after the addition, the temperature was raised to an internal temperature of 85-90°C to react for more than 1 hour. The temperature was lowered, filtered, and the filtrate was statically separated into phases. The toluene phases were combined to obtain 182.4 g of the CrDCK / toluene solution of step (2), of which CrDCK was 102.4 g and the yield was 70.0% (based on γ-butyrolactone).
[0039] Add 19...
Example Embodiment
[0040] Example 2
[0041] In a 1000mL four-necked flask, equipped with a thermometer, electric stirrer, reflux condenser, U-shaped calcium chloride drying tube. Under stirring, 80 g of toluene and 101.4 g of solid potassium tert-butoxide were added, heated to increase the internal temperature to 75° C., and 160.0 g of β-methyl-γ-butyrolactone was added dropwise. After the addition is completed, the temperature is increased to 80-90°C for reaction for 2 hours. Then, the temperature was lowered to room temperature, 402g of pre-frozen concentrated hydrochloric acid was added, and after the addition, the temperature was increased to 85~90℃ for 1 hour. The temperature was lowered, filtered, and the filtrate was statically separated into phases. In the toluene phase, 319.3g of the β-methyl-CrDCK / toluene solution of step (2) was obtained, of which CrDCK was 219.3g, and the yield was 65.0% (based on γ-butyrolactone).
[0042] Add 200g of water and 65g of solid sodium hydroxide to a 1000m...
Example Embodiment
[0043] Example 3
[0044] In a 1000mL four-necked flask, equipped with a thermometer, electric stirrer, reflux condenser, U-shaped calcium chloride drying tube. Under stirring, 90 g of toluene and 65.3 g of solid sodium ethoxide were added, heated to increase the internal temperature to 75° C., and 137.6 g of γ-butyrolactone was added dropwise. After the dripping is completed, the temperature is raised to the internal temperature of 80-90°C to react for more than 2 hours. Then, the temperature was lowered to room temperature, 402g of pre-frozen concentrated hydrochloric acid was added, and after the addition, the temperature was raised to an internal temperature of 85-90°C to react for more than 1 hour. The temperature was lowered, filtered, and the filtrate was statically separated into phases. The aqueous phase was extracted once more with 20g of toluene to wash the solid. The toluene phases were combined to obtain 209.5 g of the CrDCK / toluene solution of step (2), of which Cr...
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.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap