Preparation method and application of Syk and VEGFR2 double-target inhibitor
A compound and alkyl technology, applied in the field of preparation of dual target inhibitors of spleen tyrosine kinase and vascular endothelial growth factor 2
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[0110] The synthetic route is as follows:
[0111]
[0112] 1) Preparation of compound 2-3
[0113] The raw materials and feeding amount of step 1 are shown in Table 1 below.
[0114] Table 1
[0115]
[0116] 11.0L of dimethyl sulfoxide was added to the 50L reaction kettle, the stirring was started, the rotating speed was 150rpm, and the temperature was shown as an internal temperature of 20°C. 833.0 g of compound 2-2, 1510.0 g of N,N-diisopropylethylamine and 1100.0 g of compound 2-1 were added in this order. The external temperature was set to 100°C, and the mixture was stirred at an internal temperature of 95 to 100°C for 24 hours.
[0117] The reaction solution was detected by HPLC, and HPLC showed that compound 2-1 remained less than 3%. The heating was turned off, and the reaction solution was cooled to 20-25°C. The reaction solution was slowly poured into 30.0 L of stirred water. The internal temperature was controlled to be 10 to 15° C., and the mixture was ...
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