Phosphorus oxychloride → HCID 17963002, compound

Participants

Reaction Steps

13.5 g of 4-hydroxy-6-(4-nitrophenyl)furo[2,3-d]pyrimidine are heated for 1.5 h under RF in ca. 200 ml of phosphorus oxychloride (Fluka, Buchs). Afterwards, the reaction mixture is left to stand in the open for 3 days, and then added to 4 kg of ice. The suspension is filtered by suction and washed with a lot of H2O. The product is sublimated at ca. 200° C. and at ca. 0.1 mbar. The sublimate consists of lemon-yellow non-crystalline needles: m.p.: from 245° C. (decomposition). 1H-NMR (300 MHz, DMSO): 8.91 (s, H—C(2)); 8.40, 8.31 (d, J=9.2, H—C(2′, 3′)); 8.09 (s, H—C(5)).

Provenance & Evidence