Water → HCID 178418853, Verbindung

HRID 10517

Reaktionsgleichung

Reaktionsgleichung von HRID 10517
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:14][CH2:13][C@H:12](OS(C)(=O)=O)[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C[Si]([N:24]=[N+:25]=[N-:26])(C)C.[F-].[Cs+].O>CN(C)C=O>[C:1]([O:5][C:6]([NH:8][C@@H:9]1[CH2:14][CH2:13][C@H:12]([N:24]=[N+:25]=[N-:26])[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 25953Cesium fluorideHCID 78378AzidotrimethylsilaneHCID 178418975HCID 178418975, Verbindung

Produkt 1

HCID 178418853HCID 178418853, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of Intermediate 36 (196 g) and trimethylsilyl azide (283 ml, Tokyo Kasei Kogyo) in dimethylformamide (667 ml) was added with cesium fluoride (305 g, Wako Pure Chemical Industries) with stirring and stirred at 70° C. for 4 days. The reaction mixture was cooled to room temperature and then added twice with water in a volume of 2.75 l in total. This reaction mixture was stirred with ice cooling for 2 hours, and the deposited precipitates were collected by filtration. Then, the precipitates were washed with water to obtain a roughly purified product of the title compound (142 g).

Aufarbeitung

  1. stirringstirred at 70° C. for 4 days
  2. stirringThis reaction mixture was stirred with ice cooling for 2 hours
  3. customthe deposited precipitates
  4. filtrationwere collected by filtration
  5. washThen, the precipitates were washed with water

Quellen und Nachweise

ORD-Eintrag
ord-b811f8e37f91454ca9c82dfe2654d854
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07094789B2

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