Hydrogen Peroxide → Thieno[3,2-c]isothiazol-3-amine

HRID 2200499Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2200499
[NH2:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7](=[S:9])[NH2:8].OO>CO>[N:1]1[S:9][C:7]([NH2:8])=[C:3]2[S:4][CH:5]=[CH:6][C:2]=12

Komponenten

4

Edukt 2

HCID 784Hydrogen PeroxideHCID 143211023-Amino-2-thiophenecarbothioamide

Produkt 1

HCID 818861Thieno[3,2-c]isothiazol-3-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of crude 3-aminothiophene-2-carbothioamide in MeOH (5 mL) was added H2O2 (30%, 0.6 mL), after stirring at room temperature for 15 min, it was concentrated to remove most of MeOH, and then diluted with EtOAC, organic layer was washed with brine, concentrated to give crude pdt, purification by column chromatography (DCM/EtOAC=3:1) gave thieno[3,2-c]isothiazol-3-amine (334 mg).

Aufarbeitung

  1. concentrationit was concentrated
  2. customto remove most of MeOH
  3. additiondiluted with EtOAC, organic layer
  4. washwas washed with brine
  5. concentrationconcentrated
  6. customto give crude
  7. custompdt, purification by column chromatography (DCM/EtOAC=3:1)

Quellen und Nachweise

ORD-Eintrag
ord-282819540fdd48a7af87715042a2a4f2
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09359308B2

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