HRID2377133

反应详情

EQUATION

反应方程式

HRID 2377133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. waitkept for overnight
  2. filtrationThe suspension was filtered
  3. customRemoval of solvent