Carbon Tetrachloride → HCID 18925007, compound

Participants

Reaction Conditions

Reaction Steps

6-Methyl-quinazolin-4-one (350 mg, 2.18 mmol) was added to a suspension of polymer-supported triphenylphosphine (from Fluka, 3.63 g of about 3 mmol P/g resin; 10.9 mmol) in a mixture of CCl4 (3.35 g, 21.80 mmol) and 1,2 dichloroethane (10 mL). The mixture was heated to 60° C. for 2 hours and then the polymer was removed by filtration and washed with dichloroethane. The filtrate was collected in a flask containing 3-ethynyl-aniline (0.644 g, 2.18 mmol) and concentrated to 5 mL by evaporation. After 4 hours reflux under N2, followed by cooling to 20° C., the title product was collected by filtration (551 mg; 86%; M.P. 256°-257° C.; LC-MS: 260 (MH+); anal. RP-HPLC RT: 4.41 min).

Provenance & Evidence