Carbon Disulfide → HCID 178500329, Verbindung

HRID 460509

Reaktionsgleichung

Reaktionsgleichung von HRID 460509
[CH3:1][O:2][C:3](=[O:24])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([NH2:16])=[C:12]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:11]=1.[C:25](=S)=[S:26].C(=O)(O)[O-].[Na+]>N1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:24])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]2[N:16]=[C:25]([SH:26])[N:17]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:12]=2[CH:11]=1

Komponenten

5

Edukt 3

HCID 6348Carbon DisulfideHCID 516892Sodium BicarbonateHCID 120430856-(3-Phenylamino-4-aminophenyl)oxyhexanoic acid methyl ester

Produkt 1

HCID 178500329HCID 178500329, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

0.4 g of 6-(3-phenylamino-4-aminophenyl)oxyhexanoic acid methyl ester was dissolved in 5 ml of pyridine, mixed with 75 μl of carbon disulfide, and the mixture was stirred for 12 hours at 20° C. It was mixed with saturated sodium bicarbonate solution, extracted three times with ethyl acetate, the combined organic phases were washed with saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue was purified by column chromatography on silica gel. 368 mg was obtained.

Aufarbeitung

  1. extractionextracted three times with ethyl acetate
  2. washthe combined organic phases were washed with saturated sodium chloride solution
  3. customdried on sodium sulfate
  4. concentrationconcentrated by evaporation in a vacuum
  5. customThe residue was purified by column chromatography on silica gel
  6. custom368 mg was obtained

Quellen und Nachweise

ORD-Eintrag
ord-ed230bd5f3c9444c8e7d6fbed6fdc4f3
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07196202B2

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