反应详情

温度

65 °C

To a mixture of acid 4k (2.42 g, 5.75 mmol, 1.0 equiv) in CHCl3 (30 mL) was added oxalyl chloride (2.5 mL, 28.7 mmol, 5.0 equiv) followed by DMF (ca. 40 μL). The mixture was heated to 65° C. After 3 hr, the solvent was removed in vacuo and the resulting residue was taken up in CH2Cl2 (20 mL). 1-Methylpiperazine (1.3 mL, 11.5 mmol, 2.0 equiv) was added followed by Et3N (0.80 mL, 5.75 mmol, 1.0 equiv) and the solution was stirred at ambient temperature for 3 h. The solution was diluted with CH2Cl2 (20 mL) and washed with H2O and brine. After drying with MgSO4 and concentration in vacuo, the residue was purified by silica gel chromatography (5% MeOH:CH2Cl2) to provide chloride 61. MS (MH+) 432; Calculated 431.1 for C25H22ClN3O2.

1. customthe solvent was removed in vacuo
2. washwashed with H2O and brine
3. dry with materialAfter drying with MgSO4 and concentration in vacuo
4. customthe residue was purified by silica gel chromatography (5% MeOH:CH2Cl2)