Triethylamine → 2,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole

HRID 21733

Reaktionsgleichung

Reaktionsgleichung von HRID 21733
C(N(CC)CC)C.[Cl:8][C:9]1[S:10][C:11]2[C:17]([NH:18][NH2:19])=[C:16]([F:20])[CH:15]=[C:14]([Cl:21])[C:12]=2[N:13]=1.[C:22](Cl)(=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24].C(OCC)(=O)C>C1(C)C=CC=CC=1>[Cl:8][C:9]1[S:10][C:11]2[C:17]([N:18]([C:22](=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24])[NH2:19])=[C:16]([F:20])[CH:15]=[C:14]([Cl:21])[C:12]=2[N:13]=1

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 62493Pivaloyl chlorideHCID 199334672,4-Dichloro-6-fluoro-7-hydrazinobenzothiazole

Produkt 1

HCID 199334582,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

2.6 ml Triethylamine was added to a solution of 4.8 g 2,4-dichloro-6-fluoro-7-hydrazinobenzothiazole in 38 ml toluene. 2.4 ml Pivaloyl chloride was added dropwise and the mixture stirred for 2 hours at room temperature. It was then treated with ethyl acetate and washed with aqueous sodium hydrogen carbonate and water, dried over magnesium sulfate and concentrated. The residue was purified by column chromatography. Yield: 1.36 g=21% of theory

Aufarbeitung

  1. washwashed with aqueous sodium hydrogen carbonate and water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-3507dce14f7b4406b6930ba5b945d4f0
Quelldatensatz
uspto-grants-1995_06
Patentnummer
US05424443

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