HRID426358
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
To a solution of (5-benzyloxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid ethyl ester (120 g, 0.29 mol) in THF (1.2 L) was added water (240 mL), LiOH.H2O (16 g, 0.32 mol) and stirred at room temperature for 16 h. The solution was filtered and concentrated in vacuo to remove THF. The resulting thick liquid was acidified to pH 2 by adding 2N aqueous HCl solution and the white suspension was mechanically stirred for 1 h at room temperature. The wet white product was recovered after filtration and dissolved in EtOAc (500 mL). The organic layer was separated from water, dried (MgSO4) and concentrated in vacuo to obtain (5-benzyloxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid (105 g, 94%).
WORKUP
后处理
- filtrationThe solution was filtered
- concentrationconcentrated in vacuo
- customto remove THF
- additionby adding 2N aqueous HCl solution
- stirringthe white suspension was mechanically stirred for 1 h at room temperature
- customThe wet white product was recovered
- filtrationafter filtration
- dissolutiondissolved in EtOAc (500 mL)
- customThe organic layer was separated from water
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo