Synthesis
The general procedure for the synthesis of 2,4-dichloro-7-bromoquinazoline from 7-bromoquinazoline-2,4(1H,3H)-dione was as follows: 205.0 g (0.84 mol) of 7-bromo-1H-benzo[d]-1,3-oxazine-2,4-dione was suspended in 1.26 L (12.59 mol) of phosphorochloride at room temperature, followed by the addition of 71.34 mL (0.42 mol) N-ethyl diisopropylamine. The reaction mixture was heated to reflux and kept for 36 hours. Upon completion of the reaction, 193.6 g of the target product 7-bromo-2,4-dichloroquinazoline was obtained by a conventional post-processing step. The product was analyzed by HPLC/MS and showed that the (M+H)+ peak was located at 277/279, confirming the solid form.
References
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