Potassium Hydroxide → HCID 20033693, Verbindung

HRID 231679

Reaktionsgleichung

Reaktionsgleichung von HRID 231679
[SH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.[OH-].[K+].Br[C:15]1[S:19][C:18]([S:20]([NH2:23])(=[O:22])=[O:21])=[CH:17][CH:16]=1>CN(C)C=O.O>[C:9]([CH2:8][C:5]1[CH:4]=[CH:3][C:2]([S:1][C:15]2[S:19][C:18]([S:20]([NH2:23])(=[O:22])=[O:21])=[CH:17][CH:16]=2)=[CH:7][CH:6]=1)([OH:11])=[O:10]

Komponenten

6

Edukt 3

HCID 14797Potassium HydroxideHCID 12413045-Bromo-2-thiophenesulfonamideHCID 33905114-Mercaptophenylacetic acid

Produkt 1

HCID 20033693HCID 20033693, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6228DimethylformamideLösungsmittel2×

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

4-Mercaptophenylacetic acid (2.3 g) was dissolved in dimethylformamide under a nitrogen atmosphere and 1.8 g of potassium hydroxide dissolved in a minimum amount of water was added. 5-bromothiophene-2-sulfonamide (3.3 g) dissolved in dimethylformamide was added and the mixture heated at 120° C. for 2 hours. After cooling to room temperature water was added to the reaction mixture, the pH was adjusted to 8.6 and the mixture was extracted with ethyl acetate. The aqueous phase was separated and acidified, causing a solid to precipitate. The solid was collected by filtration and dried under vacuum to a weight of 3.25 g.

Aufarbeitung

  1. additionwas added
  2. additionwas added
  3. additionwas added to the reaction mixture
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe aqueous phase was separated
  6. customto precipitate
  7. filtrationThe solid was collected by filtration
  8. customdried under vacuum to a weight of 3.25 g

Quellen und Nachweise

ORD-Eintrag
ord-e9ec0aeb8d5c4266906869950d3ea639
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04847289

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