Preparation method and application of lafutidine and intermediate thereof
A technology of lafutidine and intermediates, applied in the field of chemical pharmacy, can solve the problems of low yield, low purity of lafutidine crude product, easy explosion and the like
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Embodiment 1
[0109] Preparation of Lafutidine
[0110] 1) Suspend 100 grams of compound (I) in 500 milliliters of ethanol at 20-30°C with stirring, control the temperature at 0-5°C, add 120 grams of ethanolamine, and stir at 25-30°C for 3.5 hours , add 400 g of 10% aqueous sodium hydroxide solution, and continue stirring for 3.5 hours at 25-30° C.;
[0111] 2) The above reaction mixture was evaporated under reduced pressure at 40-50° C. to remove volatile matter, 600 ml of ethyl acetate and 400 ml of water were added, stirred at 20-30° C. for 30 minutes, and allowed to stand to separate layers. The organic layer was successively washed with 400 ml of water and 300 ml of 5% brine, dried over anhydrous sodium sulfate, and filtered to obtain an ethyl acetate solution of the key intermediate compound (II);
[0112] 3) Transfer the above ethyl acetate solution to the reaction flask, add 61 g of compound (III) and stir at 35-40° C. for 5 hours. The reaction mixture was washed successively with...
Embodiment 2
[0116] Preparation of Lafutidine
[0117] 1) Suspend 100 g of compound (I) in 500 ml of methanol at 20-30°C under stirring conditions, control the temperature at 0-5°C, add 120 g of ethanolamine, and stir at 25-30°C for 3.5 hours , add 400 g of 10% aqueous sodium hydroxide solution, and continue stirring for 3.5 hours at 25-30° C.;
[0118] 2) The above reaction mixture was evaporated under reduced pressure at 40-50° C. to remove volatile matter, 600 ml of ethyl acetate and 400 ml of water were added, stirred at 20-30° C. for 30 minutes, and allowed to stand to separate layers. The organic layer was successively washed with 400 ml of water and 300 ml of 5% brine, dried over anhydrous sodium sulfate, and filtered to obtain the ethyl acetate solution of the key intermediate compound (II);
[0119] 3) Transfer the above ethyl acetate solution to the reaction flask, add 61 g of compound (III) and stir at 35-40° C. for 5 hours. The reaction mixture was washed successively with 20...
Embodiment 3
[0123] Preparation of Lafutidine
[0124] 1) Suspend 100 grams of compound (I) in 500 milliliters of ethanol at 20-30°C with stirring, control the temperature at 0-5°C, add 120 grams of ethanolamine, and stir at 25-30°C for 3.5 hours , add 400 g of 10% aqueous sodium hydroxide solution, and continue stirring for 3.5 hours at 25-30° C.;
[0125] 2) The above reaction mixture was evaporated under reduced pressure at 40-50° C. to remove volatile matter, 600 ml of isopropyl acetate and 400 ml of water were added, stirred at 20-30° C. for 30 minutes, and allowed to stand to separate layers. The organic layer was washed successively with 400 ml of water and 300 ml of 5% brine, dried over anhydrous sodium sulfate, and filtered to obtain the isopropyl acetate solution of the key intermediate compound (II);
[0126] 3) Transfer the above-mentioned isopropyl acetate solution to a reaction flask, add 61 g of compound (III) and stir at 35-40° C. for 5 hours. The reaction mixture was was...
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