A kind of preparation method of tranexamic acid
A technology of tranexamic acid and aminomethylcyclohexanecarboxylic acid, which is applied in the field of preparation of tranexamic acid, can solve the problem that the total yield is only 14%, and achieve reduced raw material consumption, high yield, and reduced operation The effect of steps
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Embodiment 1
[0034] 1. Catalytic hydrogenation
[0035] In a 2L autoclave, add 234g 4-(acetamidomethyl)benzoic acid, 1000mL deionized water, 50.9g NaOH, 23g Raney nickel, N 2 Substitution, hydrogen replacement, under the conditions of 100°C and 6MPa, react until there is no pressure drop, and then react for 3h. Cool down to room temperature, remove all remaining hydrogen, take it out with a suction filter bottle, filter, remove the catalyst, rinse the catalyst with water to obtain a cis-trans mixture of potassium salt of 4-(acetylaminomethyl)cyclohexylformate.
[0036] 2. Deprotection transformation into salt
[0037] Add 97.0g NaOH to the 4-(acetylaminomethyl) cyclohexyl formic acid potassium salt cis-trans mixture, stir to dissolve, pass N 2 , distill water at 130°C until there is almost no distillate, heat up to 200°C in an oil bath, the reaction solution gradually solidifies and dries, and continues to bake at this temperature for 16 hours to obtain a dry solid. Cool down to room te...
Embodiment 2
[0041] 1. Catalytic hydrogenation
[0042] In a 2L autoclave, add 234g 4-(acetamidomethyl)benzoic acid, 1000mL deionized water, 50.9g NaOH, 23g Raney nickel, N 2 Substitution, hydrogen replacement, under the conditions of 180°C and 15MPa, react until there is no pressure drop, and then react for 3h. Cool down to room temperature, remove all remaining hydrogen, take it out with a suction filter bottle, filter, remove the catalyst, rinse the catalyst with water to obtain a cis-trans mixture of potassium salt of 4-(acetylaminomethyl)cyclohexylformate.
[0043] 2. Deprotection transformation into salt
[0044] Add 97.0g NaOH to the 4-(acetylaminomethyl) cyclohexyl formic acid potassium salt cis-trans mixture, stir to dissolve, pass N 2 , distill water at 150°C until there is almost no distillate, heat up to 280°C in an oil bath, the reaction solution gradually solidifies and dries, and continues to bake at this temperature for 24 hours to obtain a dry solid. Cool down to room t...
Embodiment 3
[0048] 1. Hydrogenation
[0049] 2L autoclave, add 234g 4-(acetamidomethyl)benzoic acid, 1000mL deionized water, 61g NaOH, 25g Raney nickel, N 2Substitution, hydrogen replacement, at 150°C, 12MPa, react until there is no pressure drop, and then react for 3h. Cool down to room temperature, remove all remaining hydrogen, take it out with a suction filter bottle, filter, remove the catalyst, rinse the catalyst with water to obtain a cis-trans mixture of potassium salt of 4-(acetylaminomethyl)cyclohexylformate.
[0050] 2. Deprotection transformation into salt (best)
[0051] In 4-(acetamidomethyl) cyclohexyl formic acid potassium salt cis-trans mixture, add 83g NaOH, stir to dissolve, logical N 2 , Distill water at 130°C until there is almost no distillate, heat up to an oil bath at 230°C, the reaction solution gradually solidifies and dries, and continues to bake at this temperature for 18 hours to obtain a dry solid. Cool down to room temperature and add 1600mL of water, sti...
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