反应详情

H2SO4 (0.8 ml, 11.02 mmol) was added dropwise to a solution of 4-[(phenylmethyl)oxy]-1,3-benzenedicarboxylic acid (may be prepared as described in Description 48; 3 g, 11.02 mmol) in methanol (40 ml). The mixture was stirred at room temperature for 3 h before being poured into ice-water (40 ml). The precipitate was collected and added to a saturated NaHCO3 solution. The mixture was filtered to remove the insoluble residue and the pH of the filtrate was adjusted to pH=4.8 by HCl (6 mol/L). The precipitate was collected to afford crude product. The crude product was added to a silica gel column (300 g), and was eluted with dichloromethane/methanol=100:1 (3 L) to afford a mixture of 5-[(methyloxy)carbonyl]-2-[(phenylmethyl)oxy]benzoic acid and the title compound as a white solid. 1 g.

1. customThe precipitate was collected
2. additionadded to a saturated NaHCO3 solution
3. filtrationThe mixture was filtered
4. customto remove the insoluble residue
5. customThe precipitate was collected
6. customto afford crude product
7. washwas eluted with dichloromethane/methanol=100:1 (3 L)
8. customto afford