Industrial production method of high-purity esomeprazole sodium
A technology for esomeprazole sodium and a production method is applied in the field of high-purity esomeprazole sodium, can solve the problems of taking a long time, cannot be separated, and is difficult to industrially scale up production, and achieves high economic value and social benefit. , The oxidation reaction time is short, and the effect of reducing gastric acid secretion
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Embodiment 1
[0048] Preparation of esomeprazole sodium
[0049] Add 5-methoxy-2-(4-methoxy-3,5-dimethyl-2-pyridyl)methylthio-1H-benzimidazole 16g (48.6mmol) and 100mL (86.6g) toluene, stir to dissolve, add 0.15mL (8.1mmol) of water, 10g (48.6mmol) of D-diethyl tartrate and 6.9g (24.3mmol) of titanium isopropoxide, and keep the reaction at 50°C for about 1h. Add potassium carbonate 3.35g (24.3mmol), cool to 20°C, add cumene hydroperoxide 8.7g (content 85%, 48.6mmol), react at 20°C and monitor the reaction liquid by HPLC, react for about 2 hours, raw material 5 -Methoxy-2-(4-methoxy-3,5-dimethyl-2-pyridyl)methylthio-1H-benzimidazole basic reaction is completed (less than 2% raw material);
[0050] Add 20ml of methanol (15.8g) to the above reaction solution, stir for 10 minutes, filter the insoluble matter, add ammonia water to the filtrate to extract the organic layer (60ml*4), adjust the pH of the obtained ammonia solution to about 8 with acetic acid, and use ethyl acetate Extracted, then...
Embodiment 2
[0055] Preparation of esomeprazole sodium
[0056] Add 5-methoxy-2-(4-methoxy-3,5-dimethyl-2-pyridyl)methylthio-1H-benzimidazole 500g (1.52mol) and 4.5 kg toluene, stir to dissolve, add water 5.5mL (0.31mol), D-diethyl tartrate 313g (1.52mol) and titanium isopropoxide 217.5g (0.76mol), keep the reaction at 50°C for about 1h, add potassium carbonate 4.2g (0.03mol), cooled to 5°C, added cumene hydroperoxide 272g (content 85%, 1.52mol), reacted at 5°C and monitored the reaction liquid by HPLC, reacted for about 2 hours, raw material 5-methoxy -2-(4-methoxy-3,5-dimethyl-2-pyridyl)methylthio-1H-benzimidazole basic reaction is completed (less than 2% raw material);
[0057] Add 475ml (375g) of methanol to the above reaction solution, stir for 15 minutes, filter the insoluble matter, add ammonia water to the filtrate to extract the organic layer (2000ml*4), adjust the pH of the obtained ammonia solution to about 7.5 with acetic acid, and extract with ethyl acetate , and then dried,...
Embodiment 3
[0062] Preparation of esomeprazole sodium (with reference to Chinese patent CN1070489)
[0063] Add 5-methoxy-2-(4-methoxy-3,5-dimethyl-2-pyridyl)methylthio-1H-benzimidazole 500g (1.52mol) and 4L to the reaction flask Heat toluene to 54°C, stir to dissolve, add 3.55mL (0.2mol) of water, 190g (0.92mol) of D-diethyl tartrate and 129g (0.45mol) of titanium isopropoxide, and keep the reaction at 54°C for about 50 minutes , cooled to 10°C, and then 58g (0.45mol) of diisopropylethylamine was added to the solution, 272g (content 85%, 1.52mol) of cumene hydroperoxide was added, and the reaction was monitored by HPLC at 10°C. React about 3 hours, raw material 5-methoxyl group-2-(4-methoxyl group-3,5-dimethyl-2-pyridyl) methylthio-1H-benzimidazole basic reaction finishes (raw material 2 %the following);
[0064] Add ammonia water to the above reaction solution to extract the organic layer (1600ml*3), add 2000ml methyl isobutyl ketone to the obtained ammonia solution, adjust the pH to ...
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