Preparation method of pyridylquinazoline
A technology of pyridine quinazoline and halomethylpyridine, which is applied in the field of preparation of pyridine quinazoline, can solve problems such as difficulty in industrial production, 3-pyridine formaldehyde is not suitable for storage, etc., so as to reduce raw material cost, production cost, and yield high rate effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0025] Example 1
[0026] Add 66.9g (0.20mol) 2-methyl-4-(perfluoropropan-2-yl) phenyl carbamate, 12.9g sodium methoxide (0.24mol), 330g toluene into a mechanical stirring, condenser, A 500mL three-necked flask with a thermometer. After refluxing for 0.5 hours, 24.5g (0.24mol) of acetic anhydride was added, followed by refluxing for 4 hours. After the reaction was completed, the sodium carbonate aqueous solution was washed to neutrality, the water layer was separated, and the oil layer was distilled under reduced pressure to obtain 71.5 g Methyl acetyl (2-methyl-4-(perfluoropropan-2-yl)-phenyl) carbamate, content 95.5% (external standard of liquid spectrum), yield 91%.
[0027] Add 71.5g (0.182mol) methyl acetyl (2-methyl-4-(perfluoropropan-2-yl)-phenyl) carbamate and 285g chlorobenzene into a mechanical stirrer, condenser, and thermometer , A 1000mL three-necked flask with aeration device, control the reaction temperature at 55℃, pass in 15.5g (0.218mol) chlorine gas, control the...
Example Embodiment
[0030] Example 2
[0031] Add 66.9g (0.20mol) 2-methyl-4-(perfluoropropan-2-yl) phenyl carbamate, 12.9g sodium methoxide (0.24mol), 400g toluene into a mechanical stirring, condenser, A 500mL three-necked flask with a thermometer. After refluxing for 0.5 hours, 24.5g (0.24mol) of acetic anhydride was added, followed by refluxing for 4 hours. After the reaction was completed, the sodium carbonate aqueous solution was washed to neutrality, the water layer was separated, and the oil layer was distilled under reduced pressure to obtain 71.5 g Methyl acetyl (2-methyl-4-(perfluoropropan-2-yl)-phenyl) carbamate, the content is 95.8% (liquid spectrum external standard), the yield is 91.3%.
[0032] Add 71.5g (0.183mol) methyl acetyl (2-methyl-4-(perfluoropropan-2-yl)-phenyl) carbamate and 285g chlorobenzene into a mechanical stirrer, condenser, and thermometer , A 1000mL three-necked flask with aeration device, control the reaction temperature at 60℃, feed in 15.6g (0.220mol) chlorine gas...
Example Embodiment
[0035] Example 3
[0036] Add 66.9g (0.20mol) 2-methyl-4-(perfluoropropan-2-yl)phenyl carbamate, 12.9g sodium methoxide (0.24mol), 465g toluene into a mechanical stirring, condenser, A 500mL three-necked flask with a thermometer. After refluxing for 0.5 hours, 24.5g (0.24mol) of acetic anhydride was added, followed by refluxing for 4 hours. After the reaction was completed, the sodium carbonate aqueous solution was washed to neutrality, the water layer was separated, and the oil layer was distilled under reduced pressure to obtain 71.5 g Methyl acetyl (2-methyl-4-(perfluoropropan-2-yl)-phenyl) carbamate, the content is 95.5% (external standard of liquid spectrum), the yield is 91%.
[0037] Add 71.5g (0.182mol) methyl acetyl (2-methyl-4-(perfluoropropan-2-yl)-phenyl) carbamate and 430g chlorobenzene into a mechanical stirrer, condenser, and thermometer , A 1000mL three-necked flask with aeration device, control the reaction temperature at 55℃, pass in 15.5g (0.218mol) chlorine gas...
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