Desloratadine derivative and its preparation method and use
A technology of compound and alkyl, which is applied in its preparation method and in the field of medicine, desloratadine derivatives, and medicine, can solve the problems of benzazepine compounds' lack of activity and side effects, physicochemical properties, etc., and reach the receptor The effect of antagonism is obvious
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Embodiment 1
[0058]
[0059] II-1 (20g, 64mmol) was placed in a 250mL reaction flask, and CH was added 2 Cl 2 (100mL) Stir to dissolve, add triethylamine (10g, 98mmol), stir at -5°C, add Intermediate III-1 (5.6g, 71mmol) dropwise, keep the temperature and stir for 5h, TLC detection shows that the reaction is complete ( Developing agent ethyl acetate: petroleum ether=1:3).
[0060] The reaction solution was poured into 100 ml of cold water, fully shaken to separate into layers, and the organic layer was separated and washed three times in succession. The organic layer was dried with anhydrous sodium sulfate and left overnight. Filter and evaporate the solvent under reduced pressure to obtain a pale yellow solid. The obtained product was purified by silica gel column chromatography to obtain 17.5 g of white solid. The purity is 99.3% (HPLC normalization method), and the yield is 77.1%. ESI-MS: 353.1.
Embodiment 2
[0062]
[0063] II-1 (20g, 64mmol) was placed in a 250mL reaction flask, and CHCl was added 3 (100mL) Stir to dissolve, add pyridine (7.8g, 98mmol), stir at 60℃, add Intermediate III-2 (6.6g, 71mmol) dropwise, keep the temperature and stir for 4h, TLC detection shows that the reaction is complete (developing agent Ethyl acetate: petroleum ether = 1:3).
[0064] The reaction solution was poured into 100 ml of cold water, fully shaken to separate into layers, and the organic layer was separated and washed three times in succession. The organic layer was dried with anhydrous sodium sulfate and left to stand overnight. Filter and evaporate the solvent under reduced pressure to obtain a pale yellow solid. The obtained product was purified by silica gel column chromatography to obtain 5.4 g of white solid. The purity is 98.8% (HPLC normalization method), and the yield is 22.9%. ESI-MS: 367.2.
Embodiment 3
[0066]
[0067] Place II-1 (10g, 32mmol) in a 250mL reaction flask, add tetrahydrofuran (80mL) and stir to dissolve it, add potassium tert-butoxide (5.5g, 49mmol), stir in an ice-water bath at 0°C, add intermediate III dropwise -3 (3.8g, 36mmol), keep the temperature and stir for 3h, TLC detection shows that the reaction is over (developing solvent ethyl acetate: petroleum ether=1:3).
[0068] The reaction liquid was filtered to remove the solid insoluble matter, and the filtrate was poured into 200 ml of cold water and stirred, and solids precipitated. Filter, wash the filter cake with water, and dry to obtain a crude brown-yellow solid. The crude product was purified by silica gel column chromatography to obtain 10.9 g of white solid. The purity is 99.1% (HPLC normalization method), and the yield is 89.4%. ESI-MS: 381.2.
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