Novel method for fine purification of theobromine
A technology of theobromine and a new method, which is applied in the field of theobromine refining, can solve the problems of high cost, low refining rate, loss of theobromine, etc., and achieve the effect of low cost and good product quality
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Embodiment 1
[0012] In a 250ml four-necked reaction flask with stirring, add 20g of crude theobromine, 120ml of water, and 12ml of 30% liquid caustic soda, heat up to 70-80°C while stirring, and add 1g of activated carbon. Decolorize at this temperature for half an hour. Filtrate, add 0.2 g of sodium metabisulfite to the filtrate, stir and cool down to 70°C, keep at 65-70°C, acidify with concentrated hydrochloric acid to pH: 5-6, cool down to 25°C, filter, wash with deionized water until the chloride ion is qualified, Dried to obtain 18.5 grams of theobromine finished product. According to cp2005, EP4, USP27 full inspection passed.
Embodiment 2
[0014] In a 250ml four-necked reaction flask with stirring, add 20g of crude theobromine, 120ml of water, and 12ml of 30% liquid caustic soda, heat up to 70-80°C while stirring, and add 1g of activated carbon. Decolorize at this temperature for half an hour. Filtrate, add 0.3 g of sodium bisulfite to the filtrate, stir and cool down to 70°C, keep at 65-70°C, acidify with concentrated hydrochloric acid to pH: 5-6, cool down to 25°C, filter, wash with deionized water until chloride ions Qualified, and dried to obtain 18.6 grams of theobromine finished product. According to cp2005, EP4, USP27 full inspection passed.
Embodiment 3
[0016] In a 250ml four-necked reaction flask with stirring, add 20g of crude theobromine, 120ml of water, and 12ml of 30% liquid caustic soda, heat up to 70-80°C while stirring, and add 1g of activated carbon. Decolorize at this temperature for half an hour. Filter, add 0.4 g of sodium thiosulfate to the filtrate, stir and cool down to 70°C, keep at 65-70°C, acidify with concentrated hydrochloric acid to pH: 5-6, cool down to 25°C, filter, wash with deionized water until chloride ions Qualified, and dried to obtain 18.2 grams of theobromine finished product. According to cp2005, EP4, USP27 full inspection passed.
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