反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of (3-ethoxy-4-methoxy-phenyl)-(1-methyl-1H-benzotriazol-5-yl)-methanol from above and MnO2 (2.5 g, 29 mmol) in methylene chloride (40 mL) was stirred at room temperature for 18 h. More MnO2 (1.5 g) was added and kept for overnight. The suspension was filtered thru a pad of Celite. Removal of solvent gave (3-ethoxy-4-methoxy-phenyl)-(1-methyl-1H-benzotriazol-5-yl)-methanone as an off-white solid (1.12 g, 58% yield 2 step): 1H NMR (CDCl3) δ 1.49 (t, J=7 Hz, 3H, CH3), 3.97 (s, 3H, CH3), 4.17 (q, J=7 Hz, 2H, CH2), 4.36 (s, 3H, CH3), 6.91 (d, J=8 Hz, 1H, Ar), 7.40 (dd, J=2, 8 Hz, 1H, Ar), 7.50 (d, J=2 Hz, 1H, Ar), 7.62 (d, J=8 Hz, 1H, Ar), 8.04 (dd, J=2, 9 Hz, 1H, Ar), 8.44-8.45 (m, 1H, Ar).
WORKUP
后处理
- waitkept for overnight
- filtrationThe suspension was filtered
- customRemoval of solvent