A method for preparing vitamin B6 by 2-methyl-2-cyclopentenone
A technology of cyclopentenone and vitamins, which is applied in the field of pharmaceutical biochemical industry, can solve the problems of product coloration, long production cycle, environmental pollution, etc., and achieve the effects of easy operation and industrialization, high atomic economy of raw materials, and easy decolorization
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Embodiment 1
[0042] Example 1: Vitamin B 6 (I) Preparation
[0043]Add 90 grams of methanol, 13.4 grams (0.1 moles) of 2-methyl-2-cyclopentenone, 1.0 grams of potassium carbonate , the temperature was raised to 50° C., 30 g of 30% formaldehyde aqueous solution was added dropwise, and the solution was reacted at 50° C. for 5 hours to obtain a solution of compound III. Cool to -30°C, change the constant pressure dropping funnel into a gas inlet tube, and feed in the ozone produced by the ozone generator at a rate of 1.0-2.0 grams per hour. After 3 hours, take a sample for detection , after the complete conversion of compound III, nitrogen replacement was introduced for 30 minutes, and sodium sulfite was added to eliminate residual ozone until the ozone test was negative. Naturally rise to normal temperature, pass 3.5 grams of ammonia gas into it, stir and react at 20-25°C for 3 hours, recover methanol and water under reduced pressure, add 40 grams of ethanol, 18 grams of 35% concentrated h...
Embodiment 2
[0044] Example 2: Vitamin B 6 (I) Preparation
[0045] Add 100 g of methanol, 13.4 g (0.1 mol) of 2-methyl-2-cyclopentenone, 1.0 g of fluorinated Potassium, the temperature was raised to 50°C, and 30 g of 30% formaldehyde aqueous solution was added dropwise, and the solution was reacted at 50°C for 4 hours to obtain a solution of compound III. Cool to -30°C, change the constant pressure dropping funnel into a gas inlet tube, and feed in the ozone produced by the ozone generator at a rate of 1.0-2.0 grams per hour. After 3 hours, take a sample for detection , after the complete conversion of compound III, replace with nitrogen for 30 minutes, add hydrosulfite to eliminate residual ozone, until the ozone test is negative. Naturally rise to normal temperature, pass 11.5 grams of 30% ammonia methanol solution into it, stir and react at 20-25°C for 3 hours, recover methanol and water under reduced pressure, add 40 grams of ethanol, 18 grams of 35% concentrated hydrochloric acid t...
Embodiment 3
[0046] Example 3: Vitamin B 6 (I) Preparation
[0047] Add 90 g of ethanol, 13.4 g (0.1 mol) of 2-methyl-2-cyclopentenone, 1.0 g of three n Butylamine and 9.0 g of paraformaldehyde were reacted at 50° C. for 5 hours to obtain a solution of compound III. Cool to -25°C, change the constant pressure dropping funnel into a gas inlet tube, and feed in the ozone produced by the ozone generator at a rate of 1.0-2.0 grams per hour. After 3 hours, take a sample for detection , after the complete conversion of compound III, nitrogen replacement was introduced for 30 minutes, and sodium sulfite was added to eliminate residual ozone until the ozone test was negative. Naturally rise to normal temperature, pass 3.5 grams of ammonia gas into it, stir and react at 20-25°C for 3 hours, recover ethanol under reduced pressure, add 40 grams of ethanol, 18 grams of 35% concentrated hydrochloric acid, 0.6 grams of activated carbon, 55 Decolorize at -60°C for 1 hour, filter while it is hot, cool ...
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