Hydrochloric Acid → 2H,3H-1lambda6-thieno[2,3-d][1,2]thiazole-1,1,3-trione

HRID 2212238Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2212238
[S:1]([C:5]1[C:6](C(OC)=O)=[CH:7][S:8][CH:9]=1)(=[O:4])(=[O:3])[NH2:2].[CH3:14][O-:15].[Na+].Cl>CO>[O:4]=[S:1]1(=[O:3])[C:5]2[CH:6]=[CH:7][S:8][C:9]=2[C:14](=[O:15])[NH:2]1

Komponenten

5

Versuchsvorschrift

A mixture of methyl 4-sulfamoylthiophene-3-carboxylate (2.7 g, 12.2 mmol), methanol (12 mL), and a 25% methanolic solution of sodium methylate (3.6 mL) was refluxed for 48 h. The reaction mixture was cooled to room temperature and acidified with concentrated hydrochloride acid, and the precipitated product was collected and washed with water. Recrystallized from water, yielded 400 mg of the title compound. MS: 187.8 (M−1), 189.5 (M+1). 1H NMR (DMSO-d6): 8.34 (d, J=4.4 Hz, 1H), 7.705 (d, J=4.8 Hz, 1H).

Aufarbeitung

  1. customthe precipitated product was collected
  2. washwashed with water
  3. customRecrystallized from water

Quellen und Nachweise

ORD-Eintrag
ord-7b537e2b0847459fa2f532f5b070956c
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07101880B2

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