Method for synthesizing theobromine
A synthesis method, theobromine technology, applied in the direction of organic chemistry, can solve the problems of long production cycle, high production cost, low product yield, etc., and achieve the effect of reduced raw material consumption, reduced industrial waste liquid, and short process route
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Embodiment 1
[0013] Add 5.0 g (25.7 mmol) of caffeine and 48.3 g (771.9 mmol, concentration of 80%) of hydrazine hydrate solution into the container in turn, install a reflux condenser, stir and raise the temperature to 118 ° C, keep the temperature for 12 hours, then cool and filter . The filter cake was dried at 90° C. for 2 hours in a blast drying oven, and then the obtained product was dissolved in 50 ml of water. Place it in a container, stir, and cool down to 0°C in an ice-water bath. Add 2ml of concentrated sulfuric acid (98%) to the solution, and slowly add sodium nitrite at 0°C until the reaction solution turns the starch potassium iodide test paper blue. Use 30% sodium hydroxide aqueous solution to adjust the pH value to neutral, cool to room temperature, and filter. Wash the filter cake with 10 ml of water, and dry the filter cake at 90° C. for 4 hours in a blast drying oven to obtain 2.2 g of the target product, theobromine, with a yield of 47.4%.
Embodiment 2
[0015] Add 10.0 grams (51.5 mmol) of caffeine and 112.8 grams (1802.9 mmol, concentration of 80%) of hydrazine hydrate solution into a 250ml four-necked flask in sequence, add a reflux condenser, stir and heat up to 115°C, keep the reaction for 14 hours, and cool ,filter. After drying the filter cake, the obtained product was dissolved in 100 ml of water. Put it in a container, stir, cool down to 3°C in an ice-water bath, add 4ml of concentrated sulfuric acid (98%), slowly add sodium nitrite at 3°C, until the reaction solution can make the starch potassium iodide test paper turn blue, use 30% sodium hydroxide Aqueous solution, adjust the pH value to be neutral, cool to room temperature, filter, wash the filter cake with 20ml of water, and dry the filter cake to obtain 4.2 g of the target product, theobromine, with a yield of 45.3%.
Embodiment 3
[0017] Add 20.0 grams (103.0 mmol) of caffeine and 257.5 grams (4118.8 mmol, concentration of 80%) of hydrazine hydrate solution into a 500ml four-neck flask in turn, add a reflux condenser, stir and heat up to 110°C, keep warm for 16 hours, cool ,filter. Dry the filter cake in a blast drying oven at 80°C for 3 hours, then dissolve the obtained product in 200ml of water, place it in a 500ml four-necked flask, stir it mechanically, cool it down to 5°C in an ice-water bath, and add concentrated sulfuric acid (98%) 8ml, slowly add sodium nitrite at 5°C, until the reaction solution can make the starch potassium iodide test paper turn blue, adjust the pH value to neutral with 30% sodium hydroxide aqueous solution, cool to room temperature, filter, wash the filter cake with 40ml water , the filter cake was dried in a blast oven at 90°C for 4 hours to obtain 8.6 g of the target product, theobromine, with a yield of 46.3%.
[0018] The chromatographic purity of the product obtained i...
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