Phosphorus oxychloride → HCID 57419393, compound

Participants

Reaction Steps

A heterogeneous mixture of 4 (4.0 g, 17.76 mmol) and phosphorus oxychloride (125 mL) was heated to reflux. After 14 h the homogeneous solution was cooled to room temperature and concentrated in vacuo yielding a black oil. Water was added to the oil and the mixture was warmed. The resulting solid was filtered, washed with water and dried at room temperature to yield 4.22 g of a brown solid (97%). 1H NMR (200 MHz, DMSO-d6): δ 2.43 (s, 3H), 6.31 (s, 1H), 7.49 (m, 3H), 8.34 (m, 2H).

Provenance & Evidence