Purification method of benzimidazole derivatives
A purification method and technology of benzimidazole are applied in the field of purification of key intermediate benzimidazole derivatives, which can solve the problems of large amount of solvent, difficult to enlarge the scale of purification, difficult to realize and the like
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Examples
Embodiment 1
[0043] Add hydrogen chloride ethanol solution (30% w / w, 300mL) to a 500mL reaction flask equipped with a thermometer, add compound B (30.0g, 62.2mmol) in batches under stirring at room temperature, stir until the solid is completely dissolved, and heat the reaction solution to 30°C Stir for 20 hours. Thin-layer chromatography detected that compound B disappeared, and the reaction solution was concentrated to 1 / 3 of its original volume by rotary evaporation under reduced pressure. Add 200 mL of ethanol to the concentrated solution to dissolve, slowly add ammonia water (25%) under stirring to adjust the pH value to 9-10, and stir at room temperature for 12 h. Thin layer chromatography showed that the stirring was stopped after the end of the reaction. The insoluble matter was removed by filtration, and the filtrate was spin-dried to obtain 35.2 g of the crude product of Compound A as a viscous light yellow oil.
[0044]The crude product of Compound A was mixed with 70 g of sil...
Embodiment 2
[0048] Add hydrogen chloride ethanol solution (35% w / w, 3000mL) to a 5000mL reaction flask equipped with a thermometer, add compound B (301g, 622mmol) in batches under stirring at room temperature, stir until the solid is completely dissolved, and heat the reaction solution to 30°C and stir for 20 Hour. Thin-layer chromatography detected that compound B disappeared, and the reaction solution was concentrated to 1 / 3 of its original volume by rotary evaporation under reduced pressure. Add 2000 mL of ethanol to the concentrated solution to dissolve, slowly add ammonia water (25%) under stirring to adjust the pH value to 9-10, and stir at room temperature for 12 h. Thin layer chromatography showed that the stirring was stopped after the end of the reaction. The insoluble matter was removed by filtration, and the filtrate was spin-dried to obtain 354 g of the crude product of Compound A as a viscous pale yellow oil.
[0049] Add 1000mL ethanol to the crude product of Compound A, ...
Embodiment 3
[0053] Add hydrogen chloride ethanol solution (30% w / w, 60L) in the 100L glass reactor that thermometer is equipped with, add compound B (8.57Kg, 17.78mol) in batches under stirring at room temperature, stir until the solid dissolves completely, control the reaction liquid temperature not to If the temperature is higher than 30°C, after the addition, the reaction solution is heated to 30°C and stirred for 20 hours. Thin-layer chromatography detected that compound B disappeared, and the reaction solution was concentrated to 1 / 3 of its original volume by distillation under reduced pressure. Add 20L of ethanol to the concentrated solution to mix and dissolve, slowly add ammonia water (25%) under stirring to adjust the pH value to 9-10 (control the temperature of the reaction solution not to exceed 35°C during the process), and stir at room temperature for 12h. Thin layer chromatography showed that the stirring was stopped after the end of the reaction. The insoluble matter was r...
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Abstract
Description
Claims
Application Information
- IPC
- C07D401/12
- CPC
- C07D401/12
- Inventors
- 刘飞孟; 方奕华