Methanol → HCID 10194752, Verbindung

HRID 750152Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 750152
[CH3:1][O:2][C:3]([C:5]1[N:6]([CH2:30][C:31]2[CH:39]=[CH:38][C:34]3[O:35][CH2:36][O:37][C:33]=3[CH:32]=2)[C:7](=[O:29])[C:8]2[C:13]([C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[CH:12][C:11]([NH:21]CC1C=CC=CC=1)=[CH:10][CH:9]=2)=[O:4].CO.[H][H]>[C].[Pd].C1COCC1>[CH3:1][O:2][C:3]([C:5]1[N:6]([CH2:30][C:31]2[CH:39]=[CH:38][C:34]3[O:35][CH2:36][O:37][C:33]=3[CH:32]=2)[C:7](=[O:29])[C:8]2[C:13]([C:14]=1[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)=[CH:12][C:11]([NH2:21])=[CH:10][CH:9]=2)=[O:4]

Komponenten

6

Edukt 3

HCID 887MethanolHCID 69156557HCID 69156557, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 10194752HCID 10194752, VerbindungAusbeute 72,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 2-(benzo[1,3]dioxol-5-ylmethyl)-6-benzylamino-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (670 mg), 10% palladium carbon (200 mg), methanol (10 ml) and THF (10 ml) was stirred at room temperature at 4-5 atm hydrogen pressure for 48 hrs. Palladium carbon was filtered off and the filtrate was concentrated. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized (ethyl acetate-hexane) to give the title compound (400 mg).

Aufarbeitung

  1. filtrationPalladium carbon was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  4. customrecrystallized (ethyl acetate-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-afd71ddd0cb047478987b6584fe942d7
Quelldatensatz
uspto-grants-2008_07
Patentnummer
US07402595B2

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