Water → 3-amino-5-(4-fluorophenyl)thiophene-2-carboxylic Acid

HRID 460318

Reaktionsgleichung

Reaktionsgleichung von HRID 460318
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)[S:4][C:3]=1[C:14]([O:16]C)=[O:15].[OH-].[Li+].O.C1COCC1>CO>[NH2:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([F:13])=[CH:11][CH:12]=2)[S:4][C:3]=1[C:14]([OH:16])=[O:15]

Komponenten

6

Versuchsvorschrift

The mixture consisting of 500 mg of methyl 3-amino-5-(4-fluorophenyl)thiophene-2-carboxylate, 160 mg of lithium hydroxide, 2 ml of water, 2 ml of THF and 2 ml of methanol is stirred at RT for 3 days. After dilution with 15 ml of water, unhydrolyzed ester is removed by extraction with ethyl acetate. The aqueous phase is adjusted to pH 5 using hydrochloric acid and stirred, and the precipitated solid is filtered off with suction and dried.

Aufarbeitung

  1. customAfter dilution with 15 ml of water, unhydrolyzed ester is removed by extraction with ethyl acetate
  2. stirringstirred
  3. filtrationthe precipitated solid is filtered off with suction
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2c96ff4f637f4338b0e2cb3a6cd9e194
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07196114B2

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