Reaktion #1548079

Reaktionsgleichung

ester

3-[4-(2-Naphthalenylmethoxy)benzoyl]benzene acetic acid methylester

LiOH

→

residue

Ausbeute 99.3%

3-[4-(2-Naphthalenylmethoxy)benzoyl]benzene acetic acid

Ausbeute 99.3%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent is evaporated
2. 2
   workup.DISSOLUTIONthe residue is dissolved in water
3. 3
   Extraktionextracted with ethyl acetate (3×)
4. 4
   TrocknenThe extracts are dried (MgSO4)
5. 5
   Sonstigeevaporated to dryness

Vorschrift

A solution of the ester (1.29 g, 3.15 mmole) of Step A, is treated dropwise with 1N-LiOH and the mixture is stirred under nitrogen overnight. The solvent is evaporated and the residue is dissolved in water, acidified in the cold with 10% acetic acid (to pH 3) and extracted with ethyl acetate (3×). The extracts are dried (MgSO4) and evaporated to dryness. The residue (1.24 g, quantitative yield) is recrystallized by dissolving it in a relatively large volume of warm ethyl acetate-dichloromethane followed by concentrating to half volume. The precipitate is collected and dried at 45° C. in vacuo (0.610 g, 48.8%), m.p. 150°-152° C.

Quelle