Risperidone artificial antigen and preparation method thereof
A technology of artificial antigen and risperidone, which is applied in the preparation methods of peptides, chemical instruments and methods, animal/human peptides, etc., can solve the problems of expensive instruments, reduce non-specific binding, facilitate immune detection and high yield Effect
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Embodiment 1
[0043] (1.1) Preparation of risperidone hapten
[0044] (a) In a 50ml single-neck round bottom flask, add 200mg (0.49mmol) of risperidone, add 20mg (0.53mmol) of lithium aluminum hydride and 15ml of anhydrous THF, under nitrogen protection, reflux at 68°C for 18 hours; stop the reaction. After cooling to room temperature, 6.8ml of sodium hydroxide solution with a mass fraction of 38% was added, adjusted to pH=8, filtered and spin-dried to obtain 258mg of oily product; further purified by column chromatography TLC to obtain 175mg of product. Chromatographic fluid is ethyl acetate, product ratio shift value R f =0.3~0.5;
[0045] (b) Weigh 169mg (0.41mmol) of the product obtained in step (a) into a 50ml round bottom flask, add 5ml DMF, then add 141mg (0.84mmol) ethyl bromoacetate and 200mg (1.45mmol) potassium carbonate, stir to dissolve, The reaction temperature was gradually increased to 100°C and reacted for 20 hours; after the reaction, it was naturally cooled and subjected to v...
Embodiment 2
[0062] (1.1) Preparation of risperidone hapten
[0063] (a) In a 50ml single-necked round-bottom flask, add 0.30mmol risperidone, 0.30mmol lithium aluminum hydride and 10ml anhydrous THF, under nitrogen protection, reflux at 68℃ for 6 hours; stop the reaction, add 3.4ml mass after cooling Sodium hydroxide solution with a fraction of 38%, adjust pH=8, filter and spin-dry to obtain an oily product; further purify by column chromatography TLC to obtain the product; the chromatographic solution is ethyl acetate, and the product ratio is R f = 0.3 ~ 0.5; the yield is 85%.
[0064] (b) Weigh 100mg (0.24mmol) of the product obtained in step (a) into a 50ml round bottom flask, add 5ml DMF, then add 0.24mmol ethyl bromoacetate, 0.24mmol potassium carbonate, stir to dissolve, the reaction temperature gradually increased to 100 React at ℃ for 20 hours; after the reaction, cool naturally and perform vacuum distillation to obtain the crude product, which is purified by thin layer chromatography...
Embodiment 3
[0074] (1.1) Preparation of risperidone hapten
[0075] (a) In a 50ml single-necked round-bottom flask, add 100mg (0.25mmol) of risperidone, add 1mmol of lithium aluminum hydride and 10ml of anhydrous THF, under nitrogen protection, reflux for 24 hours at 68°C; stop the reaction, add 3.4 after cooling ml of sodium hydroxide solution with a mass fraction of 38%, adjusted to pH=8, filtered and spin-dried to obtain an oily product; further purified by column chromatography and TLC to obtain the product. Chromatographic fluid is ethyl acetate, product ratio shift value R f =0.3~0.5;
[0076] (b) Weigh 0.15mmol of the product obtained in step (a) into a 50ml round bottom flask, add 5ml DMF, then add 0.6mmol ethyl bromoacetate, 0.6mmol potassium carbonate, stir to dissolve, the reaction temperature is gradually increased to 100 ℃ reaction 10 Hours; After the reaction is over, cool naturally, perform vacuum distillation to obtain the crude product, which is purified by thin layer chromat...
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