N-bromobutanimide → HCID 10029197, compound

Participants

Reaction Steps

A 0.3 g quantity of 1-ethoxycarbonylmethyl-3-(3,4-dichlorobenzyl)-5-methylthieno[2,3-d]pyrimidin-2,4(1H,3H)-dione (compound IV-5) synthesized in Reference Example 6 and 0.137 g of N-bromosuccinimide were dissolved in 30 ml of anhydrous tetrachloromethane, and the mixture was refluxed for 2 hours. The solvent was distilled off under reduced pressure and the residual solid obtained was purified by silica gel column chromatography (eluent:chloroform:n-hexane=2:1) to afford 0.30 g of 1-ethoxycarbonylmethyl-3-(3,4-dichlorobenzyl)-6-bromo-5-methylthieno[2,3-d]pyrimidin-2,4(1H,3H)-dione having m.p. of 165.5° to 167° C. in a yield of 85%.

Provenance & Evidence