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Hydrochloric Acid → HCID 21845569, Verbindung

HRID 1417251
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1417251
Br.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:12]2[N:13]=[C:14]([NH2:17])[S:15][CH:16]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11].[C:18]1([CH3:28])[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=1.Cl>N1C=CC=CC=1>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:12]2[N:13]=[C:14]([NH:17][S:24]([C:21]3[CH:22]=[CH:23][C:18]([CH3:28])=[CH:19][CH:20]=3)(=[O:26])=[O:25])[S:15][CH:16]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 21845589HCID 21845589, Verbindung

Produkt 1

HCID 21845569HCID 21845569, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A mixture of 0.5 g of 4-(3,4-dimethoxy-phenyl)-thiazol-2-ylamine hydrobromide with 0.33 g of p-toluenesulfonyl chloride was stirred overnight with 2 ml of pyridine. The resulting, red colored solution was poured into 50 ml of 1N hydrochloric acid and extracted three times with 50 ml of methylene chloride each time. The organic extracts were combined, dried with magnesium sulphate and concentrated. The residue was chromatographed on 35 g of Kieselgel 60 with diethyl ether as the eluent. The product-containing fractions were concentrated, dissolved in 40 ml of 50% ethanol by the addition of a small amount of 2N sodium hydroxide solution and precipitated with 2N hydrochloric acid at pH 6. 0.4 g of N-[4-(3,4-dimethoxy-phenyl)-thiazol-2-yl]-4-methyl-benzenesulfonamide was obtained as colorless crystals.

Aufarbeitung

  1. extractionextracted three times with 50 ml of methylene chloride each time
  2. dry with materialdried with magnesium sulphate
  3. concentrationconcentrated
  4. customThe residue was chromatographed on 35 g of Kieselgel 60 with diethyl ether as the eluent
  5. concentrationThe product-containing fractions were concentrated
  6. dissolutiondissolved in 40 ml of 50% ethanol by the addition of a small amount of 2N sodium hydroxide solution
  7. customprecipitated with 2N hydrochloric acid at pH 6

Quellen und Nachweise

ORD-Eintrag
ord-91d2d65b303c4c5bb481b18544283781
Quelldatensatz
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05877193

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