A kind of method utilizing hydrocarbyl boronic acid, amine and carbon dioxide to synthesize carbamate
A carbamate and hydrocarbyl boronic acid technology, which is applied in the preparation of carbamic acid derivatives, organic chemical methods, chemical instruments and methods, etc., can solve problems such as environmental pollution and threats to life safety, and achieve good adaptability and safe reaction operations Simple, wide substrate adaptability effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0036] Add 0.5 mmol phenylboronic acid, 0.2 mmol cuprous oxide, 3 ml dichloromethane, 2.5 mmol diethylamine, 1.5 mmol boron trifluoride diethyl ether, 1.5 mmol pyridine to the autoclave, first fill 0.4 Oxygen in MPa, and then filled with carbon dioxide to make the total pressure reach 4MPa. After stirring and reacting at 80°C for 24 hours, stop heating and stirring, cool to room temperature, and slowly vent unreacted CO 2 . The reaction solution was extracted with ethyl acetate, filtered, and the solvent was removed by rotary evaporation under reduced pressure to obtain a crude product, which was then separated and purified by column chromatography to obtain the target product. The eluent of the column chromatography used was petroleum ether with a volume ratio of 20:1 : ethyl acetate mixed solvent, productive rate 61%.
Embodiment 2
[0038] Add 0.5 mmol phenylboronic acid, 0.2 mmol cuprous oxide, 3 ml dichloromethane, 2.5 mmol diethylamine, 1 mmol boron trifluoride diethyl ether, 1.5 mmol pyridine to the autoclave, and first fill 0.4 Oxygen in MPa, and then filled with carbon dioxide to make the total pressure reach 4MPa. After stirring and reacting at 80°C for 24 hours, stop heating and stirring, cool to room temperature, and slowly vent unreacted CO 2. The reaction solution was extracted with ethyl acetate, filtered, and the solvent was removed by rotary evaporation under reduced pressure to obtain a crude product, which was then separated and purified by column chromatography to obtain the target product. The eluent of the column chromatography used was petroleum ether with a volume ratio of 20:1 : ethyl acetate mixed solvent, productive rate 39%.
Embodiment 3
[0040] Add 0.5 mmol phenylboronic acid, 0.05 mmol cuprous oxide, 3 ml dichloromethane, 2.5 mmol diethylamine, 1.5 mmol boron trifluoride diethyl ether, 1.5 mmol pyridine into the autoclave, and first fill 0.2 Oxygen in MPa, and then filled with carbon dioxide to make the total pressure reach 4MPa. After stirring and reacting at 80°C for 24 hours, stop heating and stirring, cool to room temperature, and slowly vent unreacted CO 2 . The reaction solution was extracted with ethyl acetate, filtered, and the solvent was removed by rotary evaporation under reduced pressure to obtain a crude product, which was then separated and purified by column chromatography to obtain the target product. The eluent of the column chromatography used was petroleum ether with a volume ratio of 20:1 : ethyl acetate mixed solvent, productive rate 78%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More