반응 #640973

반응 방정식

4′-methyl-5-(5-trifluoromethyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester

LiOH.H2O

→

4′-methyl-5-(5-trifluoromethyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid

수율 97.0%

용매

THF

water

반응 조건

후처리

1. 1
   온도The reaction mixture was heated
2. 2
   온도to reflux for 3.5 hours
3. 3
   기타Solvent was removed under reduced pressure
4. 4
   workup.ADDITIONthe pH of the liquid residue was adjusted to 2.0 by addition of 2N aqueous HCl solution
5. 5
   추출The mixture was extracted with ethyl acetate
6. 6
   건조the combined ethyl acetate layers were dried over anhydrous Na2SO4
7. 7
   농축concentrated in vacuo

실험 절차

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).

출처