Tin atom → HCID 19035265, Verbindung

HRID 263823Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 263823
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[CH:10]=[C:9]([N+:11]([O-])=O)[C:8]([Cl:14])=[CH:7][C:6]=1[CH3:15].[Sn]>Cl.O.[OH-].[Na+]>[ClH:14].[NH2:11][C:9]1[C:8]([Cl:14])=[CH:7][C:6]([CH3:15])=[C:5]([NH:4][CH2:3][CH2:2][OH:1])[CH:10]=1

Komponenten

6

Edukt 2

HCID 5352426Tin atomHCID 19035261HCID 19035261, Verbindung

Produkt 1

HCID 19035265HCID 19035265, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313Hydrochloric AcidLösungsmittelHCID 962WaterLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

670 mg (2.9 mmol) of 2-(2'-hydroxyethyl)amino-5-chloro-4-nitrotoluene and 625 g of tin in 10 ml semiconcentrated hydrochloric acid were heated under reflux for one hour. After cooling, this mixture was diluted with 10 ml of water and 40 ml of 10 percent aqueous sodium hydroxide solution were added. The tin salt precipitate was filtered off and the filtrate was extracted 3 times with 30 ml of methylene chloride each time. After washing with water the filtrate was dried over sodium sulfate and the solvent was completely distilled away. The oily residue was received in 20 ml of methanol and reacted with an equimolar amount of hydrochloric acid.

Aufarbeitung

  1. temperatureunder reflux for one hour
  2. temperatureAfter cooling
  3. additionwere added
  4. filtrationThe tin salt precipitate was filtered off
  5. extractionthe filtrate was extracted 3 times with 30 ml of methylene chloride each time
  6. washAfter washing with water the filtrate
  7. dry with materialwas dried over sodium sulfate
  8. distillationthe solvent was completely distilled away
  9. customreacted with an equimolar amount of hydrochloric acid

Quellen und Nachweise

ORD-Eintrag
ord-f8960cedc16c480fa010a7fa6ea85a33
Quelldatensatz
uspto-grants-1997_07
Patentnummer
US05645610

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