反应详情

温度

100 °C

5-Iodo-6-methylisoquinolin-1(2H)-one (2.00 g, 7.02 mmol) was treated with phosphorous oxychloride (6.54 ml, 70.2 mmol) and the mixture stirred at 100° C. for 4 hours. The mixture was cooled and the volatiles removed in vacuo. The residue was taken up in DCM and washed twice with cold water and then twice with saturated aqueous sodium bicarbonate. The organic was dried with sodium sulfate, loaded unto silica and purified by column chromatography on silica gel using 20 to 60% EA in hexanes to give 1-chloro-5-iodo-6-methylisoquinoline (2.00 g, 93.9% yield) as a tan solid. MS (M+H)+ 303.7.

1. temperatureThe mixture was cooled
2. customthe volatiles removed in vacuo
3. washwashed twice with cold water
4. dry with materialThe organic was dried with sodium sulfate
5. custompurified by column chromatography on silica gel using 20 to 60% EA in hexanes