HRID712473
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-(benzyloxy)pyridin-2-yl)methanol (7.50 g) and MnO2 (30.00 g) in CHCl3 was heated to reflux for 90 min, and then cooled to rt. The reaction mixture was filtered. The filtrate was concentrated in vacuo and the residue was chromatographed with a silica gel column (eluting agent: 2:1 (v/v) PE/EA) to give the title compound as a pale yellow solid (5.40 g, 73.00%), HPLC: 93.00%. The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 214.6 (M+1); 1H NMR (400 MHz, CDCl3) δ: 5.26 (s, 2H), 7.34-7.47 (m, 7H), 8.41 (t, J=2.5 Hz, 1H), 10.40 (s, 1H) ppm.
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 90 min
- filtrationThe reaction mixture was filtered
- concentrationThe filtrate was concentrated in vacuo
- customthe residue was chromatographed with a silica gel column (eluting agent: 2:1 (v/v) PE/EA)