Hydrochloric Acid → 6-Bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]pyrazolo[5,1-b][1,3]thiazole

HRID 41267

Reaktionsgleichung

Reaktionsgleichung von HRID 41267
[Br:1][C:2]1[C:22](C(O)=O)=[C:5]2[S:6][CH:7]=[C:8]([C:9]3[C:14]([O:15][CH3:16])=[CH:13][C:12]([CH2:17][O:18][CH3:19])=[CH:11][C:10]=3[O:20][CH3:21])[N:4]2[N:3]=1.Cl>O1CCOCC1>[Br:1][C:2]1[CH:22]=[C:5]2[S:6][CH:7]=[C:8]([C:9]3[C:10]([O:20][CH3:21])=[CH:11][C:12]([CH2:17][O:18][CH3:19])=[CH:13][C:14]=3[O:15][CH3:16])[N:4]2[N:3]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 58223485HCID 58223485, Verbindung

Produkt 1

HCID 582234186-Bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]pyrazolo[5,1-b][1,3]thiazoleAusbeute 25 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a 1,4-dioxane (90.0 mL) solution of 6-bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]pyrazolo[5,1-b][1,3]thiazole-7-carboxylic acid (5.00 g, 11.7 mmol) was added concentrated hydrochloric acid (14.9 mL) and the mixture was heated to reflux for 13 hours. After the reaction was completed, the solvent was distilled off under reduced pressure, water (50 mL) was added to the residue, and the precipitated solid was subjected to suction filtration and dried to obtain the title compound (1.12 g, 2.92 mmol).

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 13 hours
  3. distillationthe solvent was distilled off under reduced pressure, water (50 mL)
  4. additionwas added to the residue
  5. filtrationthe precipitated solid was subjected to suction filtration
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7e5e6bca274745aa8f6228e6e192d79a
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08530504B2

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