-
Categories
-
Pharmaceutical Intermediates
-
Active Pharmaceutical Ingredients
-
Food Additives
- Industrial Coatings
- Agrochemicals
- Dyes and Pigments
- Surfactant
- Flavors and Fragrances
- Chemical Reagents
- Catalyst and Auxiliary
- Natural Products
- Inorganic Chemistry
-
Organic Chemistry
-
Biochemical Engineering
- Analytical Chemistry
-
Cosmetic Ingredient
- Water Treatment Chemical
-
Pharmaceutical Intermediates
Promotion
ECHEMI Mall
Wholesale
Weekly Price
Exhibition
News
-
Trade Service
Instructions for the preparation of 5-bromo-N-[[(2S)-1-ethylpyrrolidin-2-yl]methyl]-2,3-dimethoxybenzamide, hydrobromide
- Gather the necessary equipment and chemicals, including a 500 mL round-bottomed flask, a magnetic stirrer, a thermometer, a condenser, and a heating plate.
- Place the flask on the heating plate and add 500 mL of toluene, followed by 100 g of 2,3-dimethoxybenzene.
Stir the mixture until it is dissolved. - In a separate beaker, mix 50 g of 5-bromo-2-nitrobenzoxazole with 200 mL of toluene.
Stir the mixture until it is dissolved. - Slowly add the 5-bromo-2-nitrobenzoxazole solution to the 2,3-dimethoxybenzene solution, stirring constantly.
- Next, add 15 g of finely ground potassium carbonate to the mixture and stir for 30 minutes.
- After 30 minutes, add 50 g of (2S)-1-ethylpyrrolidine to the mixture and stir for an additional 30 minutes.
- After 30 minutes, filtrate the mixture through a bed of anhydrous sodium sulfate, and concentrate the filtrate to a volume of approximately 200 mL.
- Add 200 mL of water to the concentrated mixture and stir until the mixture is clear.
- Slowly add 200 mL of hydrobromic acid to the mixture, stirring constantly.
- Allow the mixture to cool to room temperature, then stir in 200 mL of toluene and allow the mixture to settle.
- Filter off the precipitated solid, wash it with 50 mL of toluene, and dry it under high vacuum.
- The resulting solid can be recrystallized from 50 mL of toluene and 50 mL of hexane.
- After recrystallization, obtain a pure sample of 5-bromo-N-[[(2S)-1-ethylpyrrolidin-2-yl]methyl]-2,3-dimethoxybenzamide, hydrobromide.
This is a general procedure for the preparation of 5-bromo-N-[[(2S)-1-ethylpyrrolidin-2-yl]methyl]-2,3-dimethoxybenzamide, hydrobromide.
Depending on the specific requirements of the final product, modifications to the procedure may be necessary.