2-Bromomethylnaphthalene → HCID 936893, Verbindung

HRID 1033002Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1033002
N[C:2]1[C:3](SC(C)(C)C)=[N:4][C:5](C)=[C:6](CC)[CH:7]=1.BrC[C:18]1[CH:27]=[CH:26][C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=1.[CH:28]([N:31](C(C)C)CC)(C)C>C(#N)C>[C:21]1([CH2:28][NH:31][C:3]2[CH:2]=[CH:7][CH:6]=[CH:5][N:4]=2)[C:20]2[C:25](=[CH:26][CH:27]=[CH:18][CH:19]=2)[CH:24]=[CH:23][CH:22]=1

Komponenten

5

Edukt 3

HCID 703202-BromomethylnaphthaleneHCID 81531DiisopropylethylamineHCID 10105052HCID 10105052, Verbindung

Produkt 1

HCID 936893HCID 936893, VerbindungAusbeute 62,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 3-amino-2-tert-butylthio-5-ethyl-6-methylpyridine (0.15 g, 0.67 mmol), 2-bromomethyl-napthalene (0.15 g, 0.67 mmol), diisopropylethylamine (86 mg, 0.67 mmol) in acetonitrile (5 mL) was refluxed under an atmosphere of nitrogen for 16 hours. The resultant mixture was concentrated under reduced pressure (15 (torr). The residue was subjected to column chromatography on silica gel (50, elution with 1% methanol in chloroform). Collection and concentration of appropriate fractions provided 98 mg (40%) of the napthylmethylaminopyridine.

Aufarbeitung

  1. temperaturewas refluxed under an atmosphere of nitrogen for 16 hours
  2. concentrationThe resultant mixture was concentrated under reduced pressure (15 (torr)
  3. customCollection and concentration of appropriate fractions

Quellen und Nachweise

ORD-Eintrag
ord-8809eb84f1ad4137842a7d6249b0298f
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05308854

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