Water → (5-Bromo-6-chloro-pyridin-2-yl)-(4-chloro-benzyl)-amine

HRID 1367360Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1367360
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[N:9]=2)=[CH:4][CH:3]=1.[Br:17]N1C(=O)CCC1=O.O>C(#N)C>[Br:17][C:11]1[CH:12]=[CH:13][C:8]([NH:7][CH2:6][C:5]2[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:9][C:10]=1[Cl:14]

Komponenten

5

Edukt 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 57619237(4-Chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine

Produkt 1

HCID 57619309(5-Bromo-6-chloro-pyridin-2-yl)-(4-chloro-benzyl)-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

To (4-chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine (538, 4.00 g, 0.0158 mol) in acetonitrile (66.7 mL, 1.28 mol) under an atmosphere of nitrogen, N-bromosuccinimide (2.81 g, 0.0158 mol) in acetonitrile (20 mL) was added slowly. The reaction was stirred at room temperature overnight, then poured into water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, concentrated and crystallized with ethyl acetate in hexane to give a white solid (539, 2.60 g, 95.3%).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated
  4. customcrystallized with ethyl acetate in hexane
  5. customto give a white solid (539, 2.60 g, 95.3%)

Quellen und Nachweise

ORD-Eintrag
ord-bf0341f0524f49d7bc9e557a84fa3f35
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07893075B2

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