Diisopropylethylamine → HCID 58447638, Verbindung

HRID 1036299Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1036299
[S:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:12]=[CH:11][C:10]([CH2:13][C:14]([OH:16])=O)=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.[F:17][C:18]1[CH:19]=[C:20]([C:24]2[N:29]=[CH:28][C:27]([NH2:30])=[CH:26][CH:25]=2)[CH:21]=[CH:22][CH:23]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C.O>[F:17][C:18]1[CH:19]=[C:20]([C:24]2[N:29]=[CH:28][C:27]([NH:30][C:14](=[O:16])[CH2:13][C:10]3[CH:11]=[N:12][C:7]([N:4]4[CH2:3][CH2:2][S:1][CH2:6][CH2:5]4)=[CH:8][CH:9]=3)=[CH:26][CH:25]=2)[CH:21]=[CH:22][CH:23]=1

Komponenten

8

Edukt 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 463118956-(3-Fluorophenyl)pyridin-3-amineHCID 58447828HCID 58447828, Verbindung

Produkt 1

HCID 58447638HCID 58447638, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of 2-(6-thiomorpholinopyridin-3-yl)acetic acid 219-4 (92 mg, 0.39 mmol), 6-(3-fluorophenyl)pyridin-3-amine 219-1 (73 mg, 0.39 mmol), HATU (162 mg, 0.43 mmol) and DIEA (104 μl, 0.6 mmol) in DMF (1.0 ml) was stirred at room temperature overnight. Then it was redistributed between water (30 ml) and ethyl acetate (40 ml). The organic phase was dried over Na2SO4 and concentrated by rotary evaporation. Silica gel column chromatography (with ethyl acetate/hexanes from 1:10 to 2:1 as eluent) gave N-(6-(3-fluorophenyl)pyridin-3-yl)-2-(6-thiomorpholinopyridin-3-yl)acetamide 219-5 as solid.

Aufarbeitung

  1. dry with materialThe organic phase was dried over Na2SO4
  2. concentrationconcentrated by rotary evaporation

Quellen und Nachweise

ORD-Eintrag
ord-c290fb7995cf4df59aa8440b35a38b62
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08546396B2

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