Preparation method for mecobalamine
A technology of methylcobalamin and methylation, which is applied in the field of preparation of a drug for treating peripheral neuritis, mecobalamin, can solve the problems of unfavorable industrialized production, high cost, complicated operation, etc. Low, easy-to-use effects
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Embodiment 1
[0029] Under dark red light, add 50ml of degassed and deoxygenated dimethylformamide into a 500ml three-neck bottle, pass through high-purity nitrogen protection, then add 27g of vitamin B12, and stir mechanically. 11.2 g of potassium hydroxide was added in batches, and after the addition was completed, mechanical stirring was continued for 0.5 h at 20°C. Add 3ml of iodomethane dropwise, continue the reaction for 4-5h, take an ice-salt bath until the inner temperature is -10°C, add 300ml of ice water to the reaction bottle in batches, and keep the inner temperature of the three-necked flask not higher than 0°C. After the addition, heat and stir for 1-1.5h, a large amount of solids precipitated, filtered with suction, and the filter cake was dissolved in water, and then chromatographically separated by acidic aluminum oxide column chromatography.
[0030] In this embodiment, the chromatography column developer is a mixture of acetone and water, specifically, the volume ratio of...
Embodiment 2
[0032] Under dark red light, add 50ml of degassed and deoxygenated tetrahydrofuran into a 500ml three-necked bottle, pass through high-purity nitrogen protection, then add 27g of vitamin B12, and stir mechanically. Add 10.6g of ethylenediamine in batches, after the addition is complete, continue mechanical stirring at 10°C for 0.5h, add dropwise 3ml of iodomethane, continue the reaction for 2h, take an ice-salt bath until the internal temperature is 5°C, and pour the mixture into the reaction flask in batches Add 400ml of ice water to keep the internal temperature of the three-necked bottle not higher than -5°C; after the addition, keep warm and mechanically stir for 1-1.5 hours, a large amount of solids will precipitate, filter with suction, and use acidic aluminum oxide column chromatography after the filter cake is dissolved in water Carry out chromatographic separation, column chromatography developer is dioxane. The corresponding eluate was collected and concentrated unde...
Embodiment 3
[0034] Under dark red light, add 50ml of degassed and deoxygenated dimethyl sulfoxide into a 500ml three-necked bottle, pass through high-purity nitrogen protection, then add 27g of vitamin B12, and stir mechanically. Add 12.8g of sodium hydroxide in batches, after the addition is complete, continue to stir mechanically at 40°C for 0.5h, add dropwise 3ml of dimethyl sulfate, continue the reaction for 2-2.5h, take an ice-salt bath until the inner temperature is 10°C, and add to the Add 500ml of ice water to the reaction bottle in batches, keep the internal temperature of the three-necked bottle not higher than 0°C; after adding, keep warm and stir mechanically for 1-1.5h, a large amount of solids precipitate out, filter with suction, and use the polyamide layer after the filter cake is dissolved in water The column is used for chromatographic separation, and the column chromatographic developing solvent is dioxane. The corresponding eluate was collected and concentrated under r...
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