HRID574662

反应详情

EQUATION

反应方程式

HRID 574662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of step E product, 2-f, (3.0 g, 7 mmol), ammonium formate (0.9 g, 14 mmol) and Pd/C (0.6 g) in MeOH (70 mL) was refluxed overnight. The reaction solution was filtered. The filtrate was evaporated under vacuum to obtain a residue, which was purified by silica gel chromatography by eluting with PE:EA=1:2 and DCM:MeOH=10:1 to afford the product, 2-g, (0.51 g, 21%). 1H NMR (300 MHz, CDCl3): δ4.47 (s, 2H), 6.30-6.32 (d, Hz, 1H), 7.23-7.25 (m, 11H), 8.72 (s, 1H), 9.98-10.00 (s, 1H).

WORKUP

后处理

  1. filtrationThe reaction solution was filtered
  2. customThe filtrate was evaporated under vacuum
  3. customto obtain a residue, which
  4. customwas purified by silica gel chromatography
  5. washby eluting with PE