反应详情

To a solution of (1-(4-fluorophenyl)-1H-indazol-5-yl)(phenyl)methanol (158 mg, 0.5 mmol) and (1-methoxypent-1-enyloxy)trimethylsilane (16 mmol) which was prepared using General Silyl Ketene Acetal Method A in 10 mL of dry DCM was added TiCl4 (0.5 mL of 1.0 M DCM solution, 0.5 mmol) and then stirred 1 h. The reaction was quenched with MeOH, poured into aqueous sodium bicarbonate and extracted 2× EtOAc. The organic layers were dried over MgSO4, filtered, concentrated and purified on SiO2 by MPLC using a EtOAc/hexane gradient to give 160 mg (77% yield) of methyl 2-((1-(4-fluorophenyl)-1H-indazol-5-yl)(phenyl)methyl)pentanoate. MS found: (M+H)+=417.

1. customThe reaction was quenched with MeOH
2. additionpoured into aqueous sodium bicarbonate
3. extractionextracted 2× EtOAc
4. dry with materialThe organic layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified on SiO2 by MPLC