HCID 178492049, Verbindung → HCID 43270961, Verbindung

HRID 1443838Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1443838
CN(C)CC[N:5](C)[C:6]1[CH:7]=[C:8]([N:14]2[C:18](S)=NN=[C:15]2[C:20]2C=C(C(C)C)C(O)=C[C:21]=2O)[CH:9]=[CH:10][C:11]=1OC>CO.CCOC(C)=O.[Pd]>[CH3:18][N:14]([CH2:15][CH2:20][CH3:21])[C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([NH2:5])[CH:7]=1

Komponenten

4

Edukt 1

HCID 178492049HCID 178492049, Verbindung

Produkt 1

HCID 43270961HCID 43270961, VerbindungAusbeute 116,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 21584119Ethylacetate methanolLösungsmittel

Versuchsvorschrift

A solution of 9.0 g (40.1 mmol mmol) of (2-Methoxy-5-nitro-phenyl)-methyl-propyl-amine (4) in 200 mL of MeOH/EtOAc (1:1) containing 5% w/w of Pd—C (10%) was subjected to hydrogenation (1 atm, balloon) overnight. The contents of the flask were passed through a short pad of celite and washed with EtOAc. The filtrate was evaporated under reduced pressure to give 7.7 g (92%) of crude amine 4-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine (5) of an oil.

Aufarbeitung

  1. customwas subjected to hydrogenation (1 atm, balloon) overnight
  2. washwashed with EtOAc
  3. customThe filtrate was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6283c08881984f199431bcfb50387acd
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07662813B2

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