A kind of synthetic method of methyldopa
A synthesis method and technology of methyldopa, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as the influence of environment and operating conditions, and achieve low cost, high reaction yield and mild conditions. Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0034] (A) Weigh 16.6g (0.1mol) of 3,4-dimethoxybenzaldehyde and 5.4g (0.1mol) of sodium methoxide into 150ml of dried dimethylformamide, stir to dissolve completely, and react Place the reactor in a cold water bath to control the temperature at about 20°C, weigh 14.5g (0.1mol) of methyl 2-acetamidopropionate, add it to the reactor in batches, stir the reaction, and complete the addition in at least 5 minutes. After all the addition was completed, the temperature was maintained and the reaction was stirred for 1.5h. After the reaction, add cold water to precipitate the intermediate, filter and wash the solid several times with cold water.
[0035] (B) Transfer the intermediate obtained in (A) to the reactor, add 150ml of dichloromethane to dissolve it, add 19.1g (0.1mol) of p-toluenesulfonyl chloride, 10.1g (0.1mol) of triethylamine ), after stirring and reacting for 2h, 4g of sodium borohydride was added, and the reaction was continued for 1h. After the reaction is finished...
Embodiment 2
[0039] (A) Weigh 166kg of 3,4-dimethoxybenzaldehyde and 54kg of sodium methoxide, put them into 500L of dried dimethylformamide, stir to dissolve completely, put the reactor in a cold water bath and control the temperature at 20 At about ℃, weigh 145 kg of methyl 2-acetylaminopropionate, add it into the reactor in batches, stir the reaction, and complete the addition in at least 5 minutes. After all the addition was completed, the temperature was maintained and the reaction was stirred for 2 h. After the reaction, add cold water to precipitate the intermediate, filter and wash the solid several times with cold water.
[0040] (B) Transfer the intermediate obtained in (A) to the reactor, add 500L of dichloromethane to dissolve it, add 191kg of p-toluenesulfonyl chloride and 101kg of triethylamine into the reactor, stir and react for 2.5h, then add boron Sodium hydride 4kg, continue to react for 1.3h. After the reaction is finished, add cold water and stir well, separate the l...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 
