Method for synthesizing 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropionic acid
A technology of chlorobutyryl and methylpropionic acid, which is applied in the fields of amide preparation and organic chemistry, can solve the problems of complex process, low yield, and many reaction steps, and achieve simple preparation process, low environmental pollution, and high reaction efficiency. The effect of fewer steps
Image
![Method for synthesizing 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropionic acid](https://images-eureka.patsnap.com/patent_img/9bbe6c21-d953-43b7-8e8a-24b25af6e0b2/GSB00000618008700011.PNG)
Examples
Embodiment 1
[0026] Add 16.00 grams (0.40mol) of sodium hydroxide and 150 milliliters of anhydrous methanol to a 250 milliliter three-necked flask and stir evenly, then, while stirring, 15.50 grams (0.05mol) of N-methyl-N-methoxy-2- [4-(4-Chlorobutanoyl)phenyl]-2-methylpropanamide is dissolved in 50 ml of anhydrous methanol to form a uniformly stirred solution dropwise into a three-necked flask, and after the dropwise addition is completed, stir and react at 30°C 18 hours. After the reaction was completed, anhydrous methanol was distilled off under reduced pressure, 100 ml of water and 100 ml of dichloromethane were added to the residue, the layers were separated, and the aqueous layer was extracted twice with 100 ml of dichloromethane respectively. The extracts containing the dichloromethane layer were combined, dried with anhydrous sodium sulfate, filtered, and the dichloromethane was distilled off under reduced pressure to obtain the product N-methyl-N-methoxy-2-(4-cyclopropylcarbonylbe...
Embodiment 2
[0031] Add 20.50 grams (82%, 0.30mol) of potassium hydroxide and 150 milliliters of anhydrous methanol in a 250 milliliter three-necked flask and stir evenly, then, while stirring, 15.50 grams (0.05mol) of N-methyl-N-methoxy -2-[4-(4-chlorobutyryl) phenyl]-2-methylpropanamide was dissolved in 50 milliliters of anhydrous methanol to form a stirred solution that was added dropwise to the there-necked flask, after the dropwise addition, at 20 The reaction was stirred at °C for 30 hours. After the reaction was completed, anhydrous methanol was distilled off under reduced pressure, 100 ml of water and 100 ml of dichloromethane were added to the residue, the layers were separated, and the aqueous layer was extracted twice with 100 ml of dichloromethane respectively. The extracts containing the dichloromethane layer were combined, dried with anhydrous sodium sulfate, filtered, and the dichloromethane was distilled off under reduced pressure to obtain the product N-methyl-N-methoxy-2-...
Embodiment 3
[0034]Add 20.00 grams (0.50mol) of sodium hydroxide and 150 milliliters of absolute ethanol to a 250 milliliter three-necked flask, stir well, then, while stirring, 15.50 grams (0.05mol) of N-methyl-N-methoxy-2 -[4-(4-Chlorobutyryl)phenyl]-2-methylpropanamide dissolved in 50 ml of absolute ethanol to form a uniformly stirred solution was added dropwise to the three-necked flask. The reaction was stirred for 30 hours. After the reaction was completed, absolute ethanol was distilled off under reduced pressure, 100 ml of water and 100 ml of dichloromethane were added to the residue, the layers were separated, and the aqueous layer was extracted twice with 100 ml of dichloromethane respectively. Combine the extracts containing the dichloromethane layer, dry over anhydrous sodium sulfate, filter, distill off the dichloromethane under reduced pressure to obtain the product N-methyl-N-methoxy-2-(4-cyclopropylcarbonylphenyl) - 12.65 g (0.046 mol) of 2-methylpropanamide, yield 92%.
...
PUM
Login to View More Abstract
Description
Claims
Application Information
- IPC
- C07C59/88; C07C51/06
- Inventors
- 骆成才; 张华星