反应详情

温度

70 °C

A solution of example 673B (200 mg, 0.5 mmol) in DMF (2.5 mL) was treated with N-methylpiperazine (0.3 mL, 2.7 mmol) and K2CO3 (350 mg, 2.5 mmol), heated at 70° C. for 1 hour, allowed to cool to room temperature, and partitioned between water and CH2Cl2. The organic extract was dried (Na2SO4), filtered, and the filtrate was concentrated under reduced pressure. The residue was purified via silica gel chromatography eluting with 10% MeOH in CH2Cl2: 0.1% NH4OH to give 135 mg of the title compound (63% yield). MS (ESI (+)) m/e 416.8, 418.8 (M+H)+.

1. temperatureto cool to room temperature
2. custompartitioned between water and CH2Cl2
3. extractionThe organic extract
4. dry with materialwas dried (Na2SO4)
5. filtrationfiltered
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe residue was purified via silica gel chromatography
8. washeluting with 10% MeOH in CH2Cl2