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Hydrochloric Acid → 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene-2-carboxamide

HRID 2364073
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2364073
CC1(C)[NH:7][C:6]2[CH:8]=[C:9]([C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH3:16])[S:10][C:5]=2[C:4](=[O:17])[NH:3]1.Cl>CO>[NH2:7][C:6]1[CH:8]=[C:9]([C:11]2[CH:12]=[N:13][NH:14][C:15]=2[CH3:16])[S:10][C:5]=1[C:4]([NH2:3])=[O:17]
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Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 66743505Cdc7-IN-15

Produkt 1

HCID 667430133-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene-2-carboxamideAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 2,2-dimethyl-6-(5-methyl-1H-pyrazol-4-yl)-2,3-dihydrothieno[3,2-d]pyrimidin-4(1H)-one (1.97 g, 7.51 mmol), 1 M aqueous HCl. (38 mL) and MeOH (38 mL) was stirred at 50° C. for 4 h. After removal of the solvent at reduced pressure, the organic materials were extracted with EtOAc/THF. The combined extracts were dried over Na2SO4 and filtered. After removal of the solvent at reduced pressure, the residue was purified by column chromatography (Purif, silica gel, EtOAc to 90:10 EtOAc/MeOH) to give the title compound (1.20 g, 72%) as a green solid:

Aufarbeitung

  1. customAfter removal of the solvent at reduced pressure
  2. extractionthe organic materials were extracted with EtOAc/THF
  3. dry with materialThe combined extracts were dried over Na2SO4
  4. filtrationfiltered
  5. customAfter removal of the solvent at reduced pressure
  6. customthe residue was purified by column chromatography (Purif, silica gel, EtOAc to 90:10 EtOAc/MeOH)

Quellen und Nachweise

ORD-Eintrag
ord-d365f5cec34a4d97ab8567ace77df18c
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08691828B2

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