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Potassium Carbonate → HCID 23666225, Verbindung

HRID 486610
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 486610
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:14]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)(=[O:18])=[O:17])=[CH:13][CH:12]=[CH:11][N:10]=2)=[CH:4][CH:3]=1.Cl[S:28]([OH:31])(=[O:30])=[O:29].C(=O)([O-])[O-].[K+:36].[K+]>N1C=CC=CC=1>[S:28]([O-:31])([O:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:14]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)(=[O:18])=[O:17])=[CH:13][CH:12]=[CH:11][N:10]=2)=[CH:4][CH:3]=1)(=[O:30])=[O:29].[K+:36]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 24638Chlorosulfonic acidHCID 3035714N-[2-[(4-Hydroxyphenyl)amino]-3-pyridinyl]-4-methoxybenzenesulfonamide

Produkt 1

HCID 23666225HCID 23666225, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2.0 g (5.38 mmol) of the compound of Example 6 was dissolved in 20 ml of pyridine. 800 mg (6.87 mmol) of chlorosulfonic acid (95%) was added dropwise thereto at -15° to -10° C. The temperature was slowly elevated to room temperature and the mixture was stirred for 3 days. A 1N aqueous potassium carbonate solution was added to the reaction mixture to adjust the pH to 8 to 9. The solvent was distilled off under reduced pressure. Water and ethyl acetate were added to the residue and an aqueous layer thus formed was separated, concentrated, purified by silica gel column chromatography and precipitated with methanol/dichloromethane to obtain 1.58 g of the title compound.

Aufarbeitung

  1. customat -15° to -10° C
  2. customwas slowly elevated to room temperature
  3. distillationThe solvent was distilled off under reduced pressure
  4. additionWater and ethyl acetate were added to the residue
  5. customan aqueous layer thus formed
  6. customwas separated
  7. concentrationconcentrated
  8. custompurified by silica gel column chromatography
  9. customprecipitated with methanol/dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-07c664627c514fcd9ea2dcaf1bfd2c45
Quelldatensatz
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05292758

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