Methyl morpholine oxide → HCID 18366609, Verbindung

HRID 379591Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 379591
[Br:1][C:2]1[C:10]2[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:5]=2[S:4][C:3]=1[CH:18]([OH:29])[C:19]1[N:23]([CH3:24])[C:22]2[CH:25]=[CH:26][CH:27]=[CH:28][C:21]=2[N:20]=1.C[N+]1([O-])CCOCC1>ClCCl.[Ru]([O-])(=O)(=O)=O.C([N+](CCC)(CCC)CCC)CC>[Br:1][C:2]1[C:10]2[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:5]=2[S:4][C:3]=1[C:18]([C:19]1[N:23]([CH3:24])[C:22]2[CH:25]=[CH:26][CH:27]=[CH:28][C:21]=2[N:20]=1)=[O:29]

Komponenten

5

Edukt 2

HCID 82029Methyl morpholine oxideHCID 18366606HCID 18366606, Verbindung

Produkt 1

HCID 18366609HCID 18366609, VerbindungAusbeute 58,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178419074HCID 178419074, VerbindungKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Prepared according to the method described in Example 37 step c from 5-bromo-6-[hydroxy(1-methyl-1H-benzimidazol-2-yl)methyl]-3-methyl-1-(2-methylpropyl)-thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (5.0 g), 4-methylmorpholine-N-oxide (1.84 g), powdered 4 Å sieves (5.0 g) and tetra-n-propyl-ammonium perruthenate (0.18 g) in dry dichloromethane (170 ml) with stirring at room temperature for 24 hours. After work up, the residue was purified by column chromatography over silica eluting with a gradient of 0-2% ethanol in dichloromethane to give the subtitle compound as a yellow powder (2.93 g).

Aufarbeitung

  1. customPrepared
  2. customAfter work up, the residue was purified by column chromatography over silica eluting with a gradient of 0-2% ethanol in dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-da46f104d2564f07980f85e01e57ed5c
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06300334B1

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