Acetic Acid → 3-Benzo[b]thiophen-2-yl-1H-5-indazolecarboxylic Acid

HRID 503114Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 503114
[S:1]1[C:5]([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=C(C#N)[CH:13]=3)[NH:8][N:7]=2)=[CH:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]1=2.[C:21]([OH:24])(=[O:23])[CH3:22].O.S(=O)(=O)(O)O>C(OCC)(=O)C>[S:1]1[C:5]([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=[C:22]([C:21]([OH:24])=[O:23])[CH:13]=3)[NH:8][N:7]=2)=[CH:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]1=2

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 222607323-Benzo[b]thiophen-2-yl-1H-5-indazolecarbonitrile

Produkt 1

HCID 222606653-Benzo[b]thiophen-2-yl-1H-5-indazolecarboxylic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

To 288 mg of 3-benzo[b]thiophen-2-yl-1H-5-indazolecarbonitrile were added 3 ml of glacial acetic acid, 1 ml of water and 0.8 ml of concentrated sulfuric acid, and the mixture was stirred at 110° C. for 4 hours. After standing to cool, the mixture was added with 120 ml of ethyl acetate, sequentially washed with water and brine, dried over anhydrous magnesium sulfate. After filtering the organic layer through a silica gel pat, the solvent was evaporated, to give 307 mg of the title compound as ocher yellow crystals.

Aufarbeitung

  1. temperatureto cool
  2. washsequentially washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationAfter filtering the organic layer through a silica gel pat
  5. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-bbd7f2500aab4d89826c9607d4fbeb8c
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07776890B2

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