A kind of method for preparing p-aminobenzamidine hydrochloride
A technology for aminobenzamidine hydrochloride and p-nitrobenzamidine hydrochloride is applied in the field of preparing p-aminobenzamidine hydrochloride, and can solve the problems of high equipment requirements, no practical value, difficult handling, etc. Simple and safe effect of chemical reaction
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0037] Embodiment 1 amidination reaction
[0038]
[0039] Pour 240ml of anhydrous methanol into a three-necked flask, and protect it with nitrogen gas under an ice-water bath. When the internal temperature drops to 8°C, add 80ml of thionyl chloride dropwise with magnetic stirring to ensure that the internal temperature during the dropping process is lower than 20°C. Add 24g of p-nitrobenzonitrile II under the condition of magnetic stirring after dropping, stop the nitrogen flow, stopper the bottle tightly, and stir at room temperature for 24h. Rotary evaporation under reduced pressure at 60°C to dryness gave intermediate III as light yellow solid. The solid was dissolved in 400ml of anhydrous methanol with magnetic stirring at room temperature, and 33g of excess ammonium carbonate was added openly, and the reaction was continued with stirring at room temperature for 16h. After suction filtration, the filtrate was rotary evaporated to dryness at 60°C, and the wet product w...
Embodiment 2
[0040] Embodiment 2 amidination reaction
[0041]
[0042] Pour 300ml of absolute ethanol into a three-necked flask, and protect it with nitrogen gas under an ice-water bath. When the internal temperature drops to 5°C, add 70ml of thionyl chloride dropwise with magnetic stirring to ensure that the internal temperature during the dropping process is lower than 20°C. Add 20 g of p-nitrobenzonitrile under the condition of magnetic stirring after dropping, stop the nitrogen flow, stopper the bottle tightly, and stir at room temperature for 20 h. Rotary evaporation under reduced pressure at 60°C to dryness gave intermediate III as light yellow solid. The solid was dissolved in 400ml of absolute ethanol with magnetic stirring at room temperature, and 27g of excess ammonium carbonate was added openly, and the reaction was continued with stirring at room temperature for 20h. After suction filtration, the filtrate was rotary evaporated to dryness at 60°C, and the wet product was dr...
Embodiment 3
[0043] Embodiment 3 amidination reaction
[0044] Compared with Example 2, the difference between Example 3 and Example 2 is that in this example, phosphorous trichloride is used instead of thionyl chloride in the amidination reaction, and the others remain unchanged. The yield of the final product in this example is 41%. HPLC: 82.43%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More