HRID77774

反应详情

EQUATION

反应方程式

HRID 77774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 4′-methyl-5-(5-trifluoromethyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester (3.7 mmol, 1.34 g) in 50 ml of THF was added a solution of LiOH.H2O (18.5 mmol, 776.3 mg) in 12 mL of water. The reaction mixture was heated to reflux for 3.5 hours, then cooled to room temperature. Solvent was removed under reduced pressure, and the pH of the liquid residue was adjusted to 2.0 by addition of 2N aqueous HCl solution. The mixture was extracted with ethyl acetate and the combined ethyl acetate layers were dried over anhydrous Na2SO4 and concentrated in vacuo to give 4′-methyl-5-(5-trifluoromethyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid as light yellow solid (1.25 g, 97% yield).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 3.5 hours
  3. customSolvent was removed under reduced pressure
  4. additionthe pH of the liquid residue was adjusted to 2.0 by addition of 2N aqueous HCl solution
  5. extractionThe mixture was extracted with ethyl acetate
  6. dry with materialthe combined ethyl acetate layers were dried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo