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Potassium Carbonate → HCID 21842452, Verbindung

HRID 1737240
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1737240
Cl.Cl.[NH2:3][C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=2[Cl:17])[N:7]=[C:6]([N:18]2[CH2:22][CH2:21][CH:20]([CH2:23][NH2:24])[CH2:19]2)[N:5]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:31][S:32](Cl)(=[O:34])=[O:33]>C1COCC1>[ClH:16].[NH2:3][C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=2[Cl:17])[N:7]=[C:6]([N:18]2[CH2:22][CH2:21][CH:20]([CH2:23][NH:24][S:32]([CH3:31])(=[O:34])=[O:33])[CH2:19]2)[N:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 21842411HCID 21842411, Verbindung

Produkt 1

HCID 21842452HCID 21842452, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In 40 ml of THF was dissolved 2.1 g of the free base obtained by neutralizing the compound of Example 62, followed by addition of 0.94 g of potassium carbonate and 0.78 g of methanesulfonyl chloride. The mixture was reacted at room temperature for 20 hours. The THF was removed by concentration and the residue was diluted with water and extracted with chloroform. The extract was washed with water and dried and the chloroform was distilled off. The residue was purified by silica gel column chromatography (elution with CHCl3 :MeOH=19:1) and the resulting oil, 2.3 g, was treated in the same manner as in Example 32 (Step 2) to provide the title compound. m.p. 220-230° C.

Aufarbeitung

  1. customobtained
  2. customThe mixture was reacted at room temperature for 20 hours
  3. customThe THF was removed by concentration
  4. additionthe residue was diluted with water
  5. extractionextracted with chloroform
  6. washThe extract was washed with water
  7. customdried
  8. distillationthe chloroform was distilled off
  9. customThe residue was purified by silica gel column chromatography (elution with CHCl3 :MeOH=19:1)
  10. additionthe resulting oil, 2.3 g, was treated in the same manner as in Example 32 (Step 2)

Quellen und Nachweise

ORD-Eintrag
ord-2fba83cf48c64044bff02078ca9c4e09
Quelldatensatz
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05962453

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