反应详情

温度

50 °C

To the product of EXAMPLE 91 (10 mg) in isopropanol (4 mL) and THF (1 mL) was added Cs2CO3 (10 mg). The reaction stirred for about 14 hours at 50° C. LC/MS indicated incomplete reaction and the solution was then heated to 90° C. in a pressure tube for three hours. The reaction was concentrated and then diluted with EtOAc. After washing with saturated aqueous NaHCO3 the solution was dried (Na2SO4). The concentrated residue was purified by preparative TLC on silica gel eluted with 5% methanol in CH2Cl2 affording the title compound. HPLC/MS: 558.0 (M+1), 560.0 (M+3); Rt=4.93 min.

1. customreaction
2. temperaturethe solution was then heated to 90° C. in a pressure tube for three hours
3. concentrationThe reaction was concentrated
4. additiondiluted with EtOAc
5. washAfter washing with saturated aqueous NaHCO3 the solution
6. dry with materialwas dried (Na2SO4)
7. customThe concentrated residue was purified by preparative TLC on silica gel
8. washeluted with 5% methanol in CH2Cl2 affording the title compound