反应详情

温度

60 °C

6-Methyl-pyrido[3,4-d]pyrimid-4-one (161 mg, 1.00 mmol) was added to polymer-supported triphenylphosphine (1.66 g of about 3 mmol P/g polymer; 5.0 mmol) along with CCl4 (1.54 g, 10.0 mmol) in 1,2-dichloroethane (6 mL). The reaction mixture was heated to 60° C. for 2 hours and then the resin was filtered and washed with 1,2-dichloroethane. The filtrate was collected in a flask containing 4-hydroxy-3-iodo-aniline (0.235 g, 1.00 mmol) and concentrated to 5 mL by evaporation. After 12 hours reflux under nitrogen followed by cooling to 20° C., the title product was collected by filtration (347 mg; 83%; M.P. 261-265° C.; LC-MS: 379 (MH+); anal. RP-HPLC: 3.20 min.).

1. filtrationthe resin was filtered
2. washwashed with 1,2-dichloroethane
3. customThe filtrate was collected in a flask
4. concentrationconcentrated to 5 mL by evaporation
5. temperatureAfter 12 hours reflux under nitrogen
6. temperatureby cooling to 20° C.
7. filtrationthe title product was collected by filtration (347 mg; 83%; M.P. 261-265° C.; LC-MS: 379 (MH+); anal. RP-HPLC: 3.20 min.)