反应详情

A solution of 3,4-dimethoxycyclobut-3-ene-1,2-dione (20.58 mg, 0.145 mmol) and triethylamine (81 μl, 0.579 mmol) in MeOH (483 μl) was warmed to 45° C. for 30 mins. 3,5-Dichlorobenzyl 4-(2-(methylamino)ethyl)piperidine-1-carboxylate (Example 1, step 3) (50 mg, 0.145 mmol) was added drop wise and the reaction mixture was stirred at room temperature for 18 hours. The resulting mixture was concentrated under reduced pressure and the crude oily product was dissolved in water and extracted with EtOAc. The organic portion was dried over MgSO4, filtered and solvent concentrated under reduced pressure. The crude product was suspended in MeOH and sonicated. The resulting white solid was filtered and dried to afford the title compound;

1. concentrationThe resulting mixture was concentrated under reduced pressure
2. dissolutionthe crude oily product was dissolved in water
3. extractionextracted with EtOAc
4. dry with materialThe organic portion was dried over MgSO4
5. filtrationfiltered
6. concentrationsolvent concentrated under reduced pressure
7. customsonicated
8. filtrationThe resulting white solid was filtered
9. customdried