HRID508604
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of alcohol 8b (3 g, 9.1 mmol) and 3 g of powdered 4 Å molecular sieves in 150 mL of DCM, was added PCC (2.94 g, 13.7 mmol) at room temperature. After 6 hours, the reaction mixture was filtered through a 0.75-in. pad of Celite. The filtrate was concentrated in vacuo then the residue was purified by column chromatography to afford the titled compound (2.1 g, 70%) as a white solid. mp 177.3-179.8° C. 1H NMR (300 MHz, DMSO-d6): δ 10.03 (s, 1H), 7.88 (d, J=8 Hz, 2H), 7.61-7.49 (m, 4H), 7.48-7.37 (m, 3H), 7.35-7.26 (m, 2H), 7.20 (s, 1H).
WORKUP
后处理
- filtrationthe reaction mixture was filtered through a 0.75-in
- concentrationThe filtrate was concentrated in vacuo
- customthe residue was purified by column chromatography