HCID 20583266, Verbindung → HCID 85803722, Verbindung

HRID 411219Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 411219
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N+:16]([O-])=O)=[C:6]([S:8]([CH2:11][C:12]([O:14][CH3:15])=[O:13])(=[O:10])=[O:9])[CH:7]=1.[H][H]>CO.[Pd]>[NH2:16][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][C:6]=1[S:8]([CH2:11][C:12]([O:14][CH3:15])=[O:13])(=[O:10])=[O:9]

Komponenten

5

Edukt 2

HCID 20583266HCID 20583266, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 85803722HCID 85803722, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

Palladium (10%) on carbon is added to a solution of methyl ((5-methyl-2-nitro-phenyl)sulfonyl)acetate (Preparation 37, 2.0 g) in MeOH (60 mL) and the solution is shaken on a Parr apparatus under 30 psi of hydrogen. After 3 hours the solution is filtered through Celite and the filter cake eluted with MeOH (60 mL). The combined MeOH eluant is evaporated and the remaining residue placed under high vacuum overnight to obtain 1.76 g (99%) of the title compound as a dark solid. Physical characteristics: MS (ESI+) m/z 244 (M+H).

Aufarbeitung

  1. filtrationAfter 3 hours the solution is filtered through Celite
  2. washthe filter cake eluted with MeOH (60 mL)
  3. customThe combined MeOH eluant is evaporated
  4. customplaced under high vacuum overnight

Quellen und Nachweise

ORD-Eintrag
ord-c37dd00edc08404685046128b31fa557
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06559145B2

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