Methylamine → N-(4-{2-[6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl]ethyl}benzyl)-N,N2-dimethylglycinamide

HRID 1668402Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1668402
Cl[CH2:2][C:3]([N:5]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:16]2[C:21](=[O:22])[C:20]3[S:23][C:24]([C:26]4[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=4)=[CH:25][C:19]=3[N:18]=[CH:17]2)=[CH:10][CH:9]=1)[CH3:6])=[O:4].[CH3:33][NH2:34]>CO.CN(C)C=O.C(OCC)(=O)C>[Cl:32][C:29]1[CH:30]=[CH:31][C:26]([C:24]2[S:23][C:20]3[C:21](=[O:22])[N:16]([CH2:15][CH2:14][C:11]4[CH:12]=[CH:13][C:8]([CH2:7][N:5]([CH3:6])[C:3](=[O:4])[CH2:2][NH:34][CH3:33])=[CH:9][CH:10]=4)[CH:17]=[N:18][C:19]=3[CH:25]=2)=[CH:27][CH:28]=1

Komponenten

6

Edukt 2

HCID 6329MethylamineHCID 592398302-chloro-N-(4-{2-[6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl]ethyl}benzyl)-N-methylacetamide

Produkt 1

HCID 59239845N-(4-{2-[6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl]ethyl}benzyl)-N,N2-dimethylglycinamide

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of the compound (0.12 g) obtained in Example 27, 40% methylamine in methanol solution (0.28 ml) and N,N-dimethylformamide (2 ml) was stirred at room temperature for 1 hr, diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane (1:1, volume ratio) to give the title compound (53 mg) as a colorless powder.

Aufarbeitung

  1. washwashed with water and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was recrystallized from ethyl acetate-hexane (1:1, volume ratio)

Quellen und Nachweise

ORD-Eintrag
ord-bc8166d171034202b405a64e4d4dbd83
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07989445B2

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