Preparation method of bilastine intermediate
A compound and reaction technology, applied in the field of pharmaceutical preparations, can solve the problems of complex preparation process, longer reaction steps, low yield and the like than lastine, and achieve the effects of cheap and easy-to-obtain reagents, moderate reaction temperature and low preparation cost.
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Embodiment 1
[0059] The preparation of formula II compound:
[0060] 1) In a three-necked flask, add 150g of the compound of formula I, 70.25g of 2-ethoxychloroethane, 500ml of N,N-dimethylacetamide, and 139.5g of potassium hydroxide;
[0061] 2) Raise the temperature to 80°C for reaction, when the liquid phase is controlled to raw material I<0.5%, start post-processing;
[0062] 3) Evaporate the solvent N,N-dimethylacetamide under reduced pressure, slowly add 500ml of ice water under ice bath, then extract 200ml*4 times with ethyl acetate, combine the organic layers, wash 200ml*2 times with saturated brine , combined the aqueous layers, and extracted 200ml*1 time with ethyl acetate. Combine the organic layers. Concentrate under reduced pressure to cut off flow to obtain intermediate II with a weight of 180 g and a yield of 97%.
[0063] The obtained intermediate II is subjected to high performance liquid chromatography analysis, and the collection of spectra is as follows figure 1 sho...
Embodiment 2
[0067] The preparation of formula II compound:
[0068] 1) In a three-necked flask, sequentially add 50g of the compound of formula I, 21.6g of 2-ethoxychloroethane, 250ml of N,N-dimethylacetamide, and 120g of potassium carbonate;
[0069] 2) Raise the temperature to 80°C for reaction, when the liquid phase is controlled to raw material I<0.5%, start post-processing;
[0070] 3) Evaporate the solvent N,N-dimethylacetamide under reduced pressure, slowly add 250ml of ice water under ice bath, then extract 100ml*4 times with ethyl acetate, combine the organic layers, and wash 100ml*2 times with saturated brine , combined the aqueous layers, and extracted 100ml*1 time with ethyl acetate. Combine the organic layers. Concentrate under reduced pressure to cut off flow to obtain intermediate II with a weight of 55.8 g and a yield of 90%.
[0071] The obtained intermediate II is subjected to high performance liquid chromatography analysis, and the collection of spectra is as follows...
Embodiment 3
[0075] The preparation of formula III compound:
[0076] 1) In the three-necked flask, add 100g of intermediate II in turn, add 250ml of tetrahydrofuran, cool down to 0-5°C for reaction, slowly add 105ml of concentrated hydrochloric acid dropwise, and stir overnight after dropping;
[0077] 2) Control in the liquid phase until raw material II<0.5%, and start post-processing;
[0078] 2) Evaporate the solvent tetrahydrofuran to dryness under reduced pressure, then extract 300ml*3 times with dichloromethane, combine the organic layers, wash 200ml*2 times with saturated brine, combine the aqueous layers, and extract 200ml*2 times with dichloromethane. Combine the organic layers. Concentrate under reduced pressure to cut off the flow to obtain intermediate III with a weight of 70.2 g and a yield of 96%.
[0079] The obtained intermediate III is carried out to high performance liquid chromatography analysis, and the collection of spectra is as follows image 3 shown. There are ...
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