Sodium Hydroxide → HCID 43651828, Verbindung

Temperatur

40 °C

To a solution of 2,2-difluoro-2-(4-fluorophenoxy)acetic acid ethyl ester (2.9 g, 12 mmol) in a mixture of MeOH (20 ml) and THF (10 ml) was added a solution of NaOH (1.48 g, 37 mmol) in water (10 ml). The reaction mixture was stirred 20 h at rt and 1 h at 40° C. The reaction mixture was concentrated and the remaining aqueous solution was diluted with water (10 ml) and washed with hexanes. The solution was acidified to pH 3 by adding 1N HCl and the heterogeneous mixture was extracted with ethyl acetate. The combined extracts were washed with brine and after drying over sodium sulfate, the solvent was removed to obtain 2,2-difluoro-2-(4-fluorophenoxy)acetic acid as

1. concentrationThe reaction mixture was concentrated
2. additionthe remaining aqueous solution was diluted with water (10 ml)
3. washwashed with hexanes
4. additionby adding 1N HCl
5. extractionthe heterogeneous mixture was extracted with ethyl acetate
6. washThe combined extracts were washed with brine
7. dry with materialafter drying over sodium sulfate
8. customthe solvent was removed

ORD-Eintrag

ord-5d08e059e9124c36b6c7516ff3c3e30d

Quelldatensatz

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08013186B2