Industrial preparation method of pantoprazole intermediate pyridine hydrochloride
A technology of pyridine hydrochloride and pantoprazole, applied in the field of medicine, can solve the problems of high cost, unfavorable industrial production, low yield and the like, and achieve the effects of easy handling, low price and cost reduction
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[0026] Example 1:
[0027] (1) Preparation of 3-methoxy-2-methyl-4H-pyran-4-one
[0028] Dissolve 140g of sodium hydroxide in 250g of water, then add 141g of maltol, stir to dissolve, heat to 84°C, slowly add 19g of dimethyl sulfate dropwise, and control the temperature at 84~85°C, and use 30 % Sodium hydroxide solution adjusts the pH value to be maintained at about 11. After the dripping is completed, the temperature is raised to 96°C, kept for 13 hours, and the temperature is lowered to below 30°C to obtain 130g of orange-yellow liquid of 3-methoxy-2-methyl-4H-pyridine Pyran-4one;
[0029] (2) Preparation of 3-methoxy-2-methyl-4(1H)-pyridone
[0030] Add 140g of 3-methoxy-2-methyl-4H-pyran-4one to 1700g of ammonia water, stir at 85°C for 16 hours, and then evaporate under reduced pressure to remove water and dry to obtain 130g of finished product as a brown-yellow solid 3-methoxy- 2-Methyl-4(1H)-pyridone, the yield is 93%;
[0031] (3) Preparation of 4-chloro-3-methoxy-2-methylpyri...
Example Embodiment
[0041] Example 2:
[0042] (1) Preparation of 3-methoxy-2-methyl-4H-pyran-4-one
[0043] Dissolve 230g of sodium hydroxide in 410g of water, then add 231g of maltol, stir to dissolve, heat up to 84℃, slowly add 312g of dimethyl sulfate dropwise, the temperature of the drop is controlled at 80°C, and 30% hydrogen is used at the end of the drop Adjust the pH value of the sodium oxide solution to keep around 11, after the dropping, the temperature is raised to 92°C, kept for 13 hours, and the temperature is lowered to below 30°C to obtain 210g of orange-yellow liquid 3-methoxy-2-methyl-4H-pyran -4 Ketones;
[0044] (2) Preparation of 3-methoxy-2-methyl-4(1H)-pyridone
[0045] Add 210g of 3-methoxy-2-methyl-4H-pyran-4one to 2550g of ammonia, stir at 80°C for 16 hours, and then evaporate under reduced pressure to remove water and dry to obtain the finished product 198g of brown-yellow solid 3-methoxy -2-Methyl-4(1H)-pyridone, the yield is 93.9%;
[0046] (3) Preparation of 4-chloro-3-meth...
Example Embodiment
[0056] Example 3:
[0057] (1) Preparation of 3-methoxy-2-methyl-4H-pyran-4-one
[0058] Dissolve 160g of sodium hydroxide in 285g of water, add 159g of maltol, stir to dissolve, heat to 86°C, slowly add 218g of dimethyl sulfate dropwise, the temperature of the drop is controlled at 85°C, and 30% hydrogen is used in the later stage of the drop Adjust the pH value of the sodium oxide solution to keep around 11, after the dripping, the temperature is raised to 96°C, kept for 13 hours, and the temperature is lowered to below 30°C to obtain 148g of orange-yellow liquid 3-methoxy-2-methyl-4H-pyran -4 Ketones;
[0059] (2) Preparation of 3-methoxy-2-methyl-4(1H)-pyridone
[0060] Add 175g of 3-methoxy-2-methyl-4H-pyran-4one to 2100g of ammonia, stir at 85°C for 16 hours, and then evaporate under reduced pressure to remove water and dry to obtain the finished product 164g of brown solid 3-methoxy -2-Methyl-4(1H)-pyridone, the yield is 93.5%;
[0061] (3) Preparation of 4-chloro-3-methoxy-2-...
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