Hydrazine → 4-Methyl-3-(7-oxo-6,7-dihydrothieno[2,3-d]pyridazin-2-yl)benzoic acid

HRID 886761Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 886761
C([NH:5][C:6]([C:8]1[S:12][C:11]([C:13]2[CH:14]=[C:15]([CH:19]=[CH:20][C:21]=2[CH3:22])[C:16]([OH:18])=[O:17])=[CH:10][C:9]=1[CH:23]=O)=[O:7])(C)(C)C.[NH2:25]N>C(O)(=O)C>[CH3:22][C:21]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=[O:17])=[CH:14][C:13]=1[C:11]1[S:12][C:8]2[C:6](=[O:7])[NH:5][N:25]=[CH:23][C:9]=2[CH:10]=1

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 866181953-(5-(Tert-butylcarbamoyl)-4-formylthiophen-2-yl)-4-methylbenzoic acid

Produkt 1

HCID 685622714-Methyl-3-(7-oxo-6,7-dihydrothieno[2,3-d]pyridazin-2-yl)benzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A solution of 3-(5-(tert-butylcarbamoyl)-4-formylthiophen-2-yl)-4-methylbenzoic acid (2.30 g, 6.7 mmol) in acetic acid (20 ml) was treated with hydrazine (0.73 ml, 20 mmol) and heated to 110° C. for 8 hrs. After cooling to RT the volatiles were removed in vacuo. The residue was recrystallized from MeOH. Yield: 1.01 g. MS (ESI, pos. ion) m/z: 287 (M+1).

Aufarbeitung

  1. temperatureAfter cooling to RT the volatiles
  2. customwere removed in vacuo
  3. customThe residue was recrystallized from MeOH

Quellen und Nachweise

ORD-Eintrag
ord-6cfa6e3f10504266b9b609d16d646398
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08247409B2

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