反应详情

The product of EXAMPLE 54 (30 mg) in THF (2.5 mL) was combined with sodium hydride (5 mg, 60% in mineral oil). The suspension was stirred for 10 min were upon iodomethane (37 uL) was added. The reaction was stirred for about 6.5 hours at room temperature. The reaction mixture was quenched with saturated aqueous NaHCO3 and diluted with EtOAc. The EtOAc solution was dried (Na2SO4). The concentrated residue was purified by preparative TLC on silica gel eluted with 35% EtOAc in hexane affording the title compound. HPLC/MS: 486.2 (M+1), 488.2 (M+3); Rt=4.72 min.

1. additionwas added
2. stirringThe reaction was stirred for about 6.5 hours at room temperature
3. customThe reaction mixture was quenched with saturated aqueous NaHCO3
4. additiondiluted with EtOAc
5. dry with materialThe EtOAc solution was dried (Na2SO4)
6. customThe concentrated residue was purified by preparative TLC on silica gel
7. washeluted with 35% EtOAc in hexane affording the title compound