반응 #55184

반응 방정식

3-(2',4'-difluoro-4-biphenylyl)-3-hydroxybutyric acid ethyl ester

HCl

SOCl2

→

3-(2',4'-difluoro-4-biphenylyl)butyric acid

용매

dichloromethane

반응 조건

후처리

1. 1
   온도The mixture is warmed to 50° for 2 hours
2. 2
   기타solvent is removed
3. 3
   workup.DISSOLUTIONThe residue, 3'(2',4'-difluoro-4-biphenylyl)-3-chlorobutyric acid ethyl ester, is dissolved in 100 ml
4. 4
   기타at 25°
5. 5
   여과The precipitate is filtered off
6. 6
   workup.ADDITIONof water is added to the filtrate
7. 7
   온도The mixture is heated
8. 8
   온도under reflux for 2 hours
9. 9
   기타evaporated
10. 10
    workup.DISSOLUTIONthe residue is dissolved in water

실험 절차

A solution of 3.2 g. of 3-(2',4'-difluoro-4-biphenylyl)-3-hydroxybutyric acid ethyl ester in 10 ml. of dichloromethane is saturated with dry HCl gas and 1 ml. of SOCl2 is added. The mixture is warmed to 50° for 2 hours and solvent is removed. The residue, 3'(2',4'-difluoro-4-biphenylyl)-3-chlorobutyric acid ethyl ester, is dissolved in 100 ml. of methanol and hydrogenated on 100 mg. of platinum oxide under normal pressure at 25°. The precipitate is filtered off. A solution of 0.4 g. of NaOH in 5 ml. of water is added to the filtrate. The mixture is heated under reflux for 2 hours and evaporated and the residue is dissolved in water and worked up in the customary manner to give 3-(2',4'-difluoro-4-biphenylyl)butyric acid, m.p. 109°-110°.

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