Hydrochloric Acid → HCID 59536813, Verbindung

HRID 220680Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 220680
[CH2:1]([NH:4][C:5]([NH:7][NH:8][C:9](=O)[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=1[Br:17])=[O:6])[CH:2]=[CH2:3].[OH-].[Na+].Cl>>[CH2:1]([N:4]1[C:9]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[Br:17])=[N:8][NH:7][C:5]1=[O:6])[CH:2]=[CH2:3]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59536782HCID 59536782, Verbindung

Produkt 1

HCID 59536813HCID 59536813, Verbindung

Versuchsvorschrift

Of the compound from Example 163A, 11.3 g (33.98 mmol) were taken up in 61 ml (183.47 mmol) of 3M aqueous sodium hydroxide solution and heated under reflux for 36 h. The batch was then cooled, the fine precipitate was removed by filtration, and the filtrate was admixed, with ice cooling, with 28 ml (169.88 mmol) of half-concentrated hydrochloric acid to a pH of 10. The batch was filtered with suction and the product was dissolved out of the precipitate using methanol. The methanol was removed on a rotary evaporator. The residue was dried in an HV. This gave 9.78 g (69% of theory) of the title compound in 75% purity.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 36 h
  3. temperatureThe batch was then cooled
  4. customthe fine precipitate was removed by filtration
  5. filtrationThe batch was filtered with suction
  6. dissolutionthe product was dissolved out of the precipitate
  7. customThe methanol was removed on a rotary evaporator
  8. customThe residue was dried in an HV

Quellen und Nachweise

ORD-Eintrag
ord-4c4615ca118b4ed6bb8e63aa027fcbe5
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08202895B2

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