ethyl 4-bromo-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylate synthesis

Yield:1029144-28-2 80%

Reaction Conditions:

Stage #1: C₉H₉N₃O₃with phosphorus(V) oxybromide at 90; for 1 h;
Stage #2: with water;sodium hydrogencarbonate at 0; for 0.5 h;

Steps:

6.B

Step B; To a heated solution of POBr₃ (100 g) the title compound from Step A above (14.5 g), was added. The suspension was heated to 9O⁰C for 1 h. After cooled to room temperature, the resulting residue was added in small portions to an ice cooled saturated aqueous solution OfNaHCO₃ (3.5 1). After stirring for 30 min. the suspension was filtered. The resulting solid was washed with water and dried to afford the title compound as a off-white solid (15.2 g; 80 %; MH⁺ = 270/272).

References:

WO2008/63669,2008,A1 Location in patent:Page/Page column 74