Ethanol → HCID 11978594, Verbindung

HRID 1851427Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1851427
[C:1]([C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:15])=[O:14])#[N:2].N[CH2:22][CH2:23][SH:24].C(O)C>O>[S:24]1[CH2:23][CH2:22][N:2]=[C:1]1[C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:14])=[O:15]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 6058CysteamineHCID 57901755HCID 57901755, Verbindung

Produkt 1

HCID 11978594HCID 11978594, VerbindungAusbeute 29,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of N-(2-cyano-1H-indol-7-yl)thiophene-2-sulfonamide (0.54 g), 2-aminoethanethiol (0.14 g) and ethanol (20 mL) was stirred at 60° C. overnight. Water was added to the reaction mixture, and the obtained crystals were filtrated, washed with water and dried. The obtained crystals were subjected to silica gel column chromatography, and eluted with ethyl acetate. The eluate was treated with activated carbon and concentrated to give the title compound (0.19 g, yield 29%) as colorless crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point 189-190° C.

Aufarbeitung

  1. filtrationthe obtained crystals were filtrated
  2. washwashed with water
  3. customdried
  4. washeluted with ethyl acetate
  5. additionThe eluate was treated with activated carbon
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-2b76a62c22b84eea8cf4a66740f73062
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08957070B2

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