反应详情

To a solution of (4-(5-bromo-2-chlorobenzyl)phenyl)methanol (intermediate AK) (1 g) in CH2Cl2 (10 mL), the solution of Dess-Martin periodinane (DMP) (1.22 g) CH2Cl2 (10 mL) was added dropwise. 0° C. The mixture was warmed to room temperature, and the reaction was monitored by TLC. After 1 h, CH2Cl2 was added to dilute the solution and 1 M NaOH was added to quench the reaction. The CH2Cl2 layer was separated and washed with aqueous NaHSO3 and brine, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AL (0.62 g).

1. custom0° C
2. additionwas added
3. customto quench
4. customthe reaction
5. customThe CH2Cl2 layer was separated
6. washwashed with aqueous NaHSO3 and brine
7. dry with materialdried over Na2SO4
8. customThe solvent was evaporated under reduced pressure
9. customthe product was purified by column chromatography
10. customto obtain pure intermediate AL (0.62 g)