Methanol → 5-(3-Chloro-benzoylamino)-2-phenoxy-benzoic acid

5-(3-Chloro-benzoylamino)-2-phenoxy-benzoic acid methyl ester (1.56 g, 4.00 mmol) (see Example I1) was dissolved in a mixture of tetrahydrofuran (15 ml), methanol (1.5 ml), and water (1.5 ml). Lithium hydroxide monohydrate (336 mg, 8 mmol) was added and the reaction mixture stirred at ambient temperature for 3 days. The reaction mixture was concentrated and the residue extracted with water and tert-butyl-methyl-ether. The aqueous phase was acidified by the addition of a few drops of concentrated hydrochloric acid and extracted with ethyl acetate. The phases were separated, the organic phase was dried over sodium sulfate and concentrated. The residue was used without further purification.

1. concentrationThe reaction mixture was concentrated
2. extractionthe residue extracted with water and tert-butyl-methyl-ether
3. additionThe aqueous phase was acidified by the addition of a few drops of concentrated hydrochloric acid
4. extractionextracted with ethyl acetate
5. customThe phases were separated
6. dry with materialthe organic phase was dried over sodium sulfate
7. concentrationconcentrated
8. customThe residue was used without further purification

ORD-Eintrag

ord-69d1285ae438474e930e547087e95976

Quelldatensatz

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08420855B2