Hydrochloric Acid → HCID 19374875, Verbindung

HRID 128690Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 128690
Cl.C([NH:10][C:11](=[S:25])[N:12]([CH:16]([C:18]1[CH:23]=[CH:22][N:21]=[CH:20][C:19]=1[Cl:24])[CH3:17])[CH2:13][CH2:14][CH3:15])(=O)C1C=CC=CC=1>O>[Cl:24][C:19]1[CH:20]=[N:21][CH:22]=[CH:23][C:18]=1[CH:16]([N:12]([CH2:13][CH2:14][CH3:15])[C:11]([NH2:10])=[S:25])[CH3:17]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 19374853HCID 19374853, Verbindung

Produkt 1

HCID 19374875HCID 19374875, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Add 6 ml of 32% hydrochloric acid to 1.18 g of the compound obtained in Step A. Bring the reaction medium to 80° C. for one hour, then cool and add water. Extract with methylene chloride and discard the organic phase. Alkanilise the aqueous phase with sodium carbonate and extract with methylene chloride. Dry the organic phase and evaporate under vacuum. Purify the residue by chromatography on a silica column, using a mixture of methylene chloride and methanol (98:2 V/V) as eluent.

Aufarbeitung

  1. temperaturecool
  2. extractionExtract with methylene chloride
  3. extractionAlkanilise the aqueous phase with sodium carbonate and extract with methylene chloride
  4. customDry the organic phase
  5. customevaporate under vacuum
  6. customPurify the residue by chromatography on a silica column
  7. additiona mixture of methylene chloride and methanol (98:2 V/V) as eluent

Quellen und Nachweise

ORD-Eintrag
ord-0a6fbf346934482d880efff9a5832b05
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05464847

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