HCID 86614812, Verbindung → HCID 86614818, Verbindung

HRID 1686157Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1686157
[CH3:1][C:2]1[C:10]([CH3:19])([CH2:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=[O:17])=[O:16])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([S:20]([O-:23])(=[O:22])=[O:21])[CH:8]=2)[N:3]=1.[Na+:24].[Na+]>C1COS(=O)(=O)CC1>[CH3:1][C:2]1[C:10]([CH3:19])([CH2:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=[O:16])=[O:17])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([S:20]([O-:23])(=[O:21])=[O:22])[CH:8]=2)[N+:3]=1[CH2:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=[O:17])=[O:16].[Na+:24].[Na+:24]

Komponenten

3

Edukt 1

HCID 86614812HCID 86614812, Verbindung

Produkt 1

HCID 86614818HCID 86614818, VerbindungAusbeute 217,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 154111,4-Butane sultoneLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

Disodium 2,3-dimethyl-3-(4-sulphonatobutyl)-3H-indole-5-sulphonate (1.0 g) and 1,4-butanesultone (10 ml) were mixed and heated under nitrogen at 150° C. for 52 hrs to give a dark purple slurry. After cooling, the mixture was triturated with ethyl acetate: the solid portion was collected by filtration, washed with ethyl acetate and diethyl ether, then dried under high vacuum over phosphorus pentoxide to give the title product (1.45 g), which was used directly without purification.

Aufarbeitung

  1. customto give a dark purple slurry
  2. temperatureAfter cooling
  3. customthe mixture was triturated with ethyl acetate
  4. filtrationthe solid portion was collected by filtration
  5. washwashed with ethyl acetate and diethyl ether
  6. dry with materialdried under high vacuum over phosphorus pentoxide

Quellen und Nachweise

ORD-Eintrag
ord-b865b0f68dc94353ac068be4a51a97f3
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08148539B2

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