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Ethanolamine → HCID 58504053, Verbindung

HRID 2407811
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2407811
[NH2:1][C:2]1[C:7]([Cl:8])=[C:6](Cl)[N:5]=[C:4]([C:10]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][N:17]([CH2:20][C:21]3[S:25][C:24]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=4)=[N:23][CH:22]=3)[CH2:16][CH2:15]2)=[O:11])[CH:3]=1.[NH2:32][CH2:33][CH2:34][OH:35]>CC(N(C)C)=O>[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([NH:32][CH2:33][CH2:34][OH:35])[N:5]=[C:4]([C:10]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][N:17]([CH2:20][C:21]3[S:25][C:24]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=4)=[N:23][CH:22]=3)[CH2:16][CH2:15]2)=[O:11])[CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 700EthanolamineHCID 585039374-amino-5,6-dichloro-N-((1-((2-(pyridin-2-yl)thiazol-5-yl)methyl)piperidin-4-yl)methyl)picolinamide

Produkt 1

HCID 58504053HCID 58504053, VerbindungAusbeute 56,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

The compound prepared in Example 407 (0.065 g) and 2-aminoethanol (0.008 g) were suspended in dimethyl acetamide (3 mL) and heated at 160° C. for 30 minutes. The reaction mixture was heated at 200° C. for 1 hour. The reaction mixture was cooled to room temperature and partitioned between saturated aqueous sodium bicarbonate and ethyl acetate. The organics were washed with brine, dried, magnesium sulfate and concentrated under reduced pressure to afford the crude material. The crude material was purified by flash column chromatography (eluant: 1-4% (9:1=methanol:ammonium hydroxide)/ethyl acetate) to furnish the title compound (0.037 g), possessing the following physical data.

Aufarbeitung

  1. temperatureThe reaction mixture was heated at 200° C. for 1 hour
  2. temperatureThe reaction mixture was cooled to room temperature
  3. custompartitioned between saturated aqueous sodium bicarbonate and ethyl acetate
  4. washThe organics were washed with brine
  5. customdried
  6. concentrationmagnesium sulfate and concentrated under reduced pressure
  7. customto afford the crude material
  8. customThe crude material was purified by flash column chromatography (eluant: 1-4% (9:1=methanol:ammonium hydroxide)/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-d63403cb37624e05853f07bbfe8c589e
Quelldatensatz
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08809538B2

Notizen zur Reaktion

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