反应详情

温度

120 °C

To a solution of 0.2 g (0.60 mmol) of (4E)-6-iodo-4-(methoxymethylene)isoquinoline-1,3(2H,4H)-dione in 2 mL of N,N′-dimethylformamide is added 4-piperidin-1-ylmethyl-phenylamine (0.127 mL, 0.67 mmol). The reaction mixture is heated at 120° C. under N2 for 1.5 h. After cooling, ethyl ether is added and left in refrigerator overnight to give dark brown crystal. The crystal is collected and dissolved in 4 mL of dimethyl sulfoxide, followed by addition of 6 mL of 65% MeOH/H2O solution to give a precipitate. The solid is collected and washed thoroughly with water, MeOH, Et2O and hexane, and air-dried to give 0.143 g (48.3% yield) of tan solid: mp 202-203° C., MS (ESI) m/z 488.1 (M+H)+1

1. temperatureAfter cooling
2. customto give dark brown crystal
3. customThe crystal is collected
4. dissolutiondissolved in 4 mL of dimethyl sulfoxide
5. additionfollowed by addition of 6 mL of 65% MeOH/H2O solution
6. customto give a precipitate
7. customThe solid is collected
8. washwashed thoroughly with water, MeOH, Et2O and hexane
9. customair-dried