Triethylamine → HCID 9888514, Verbindung

HRID 2120172Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2120172
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[C:16]([NH:17][CH2:18][CH:19]3[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]3)=[CH:15][CH:14]=[CH:13][N:12]=2)=[O:10])=[N:6][CH:7]=1.Cl.Cl[C:27]1[CH:32]=[CH:31][N:30]=[CH:29][CH:28]=1.C(N(CC)CC)C>CCO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[C:16]([NH:17][CH2:18][CH:19]3[CH2:20][CH2:21][N:22]([C:27]4[CH:32]=[CH:31][N:30]=[CH:29][CH:28]=4)[CH2:23][CH2:24]3)=[CH:15][CH:14]=[CH:13][N:12]=2)=[O:10])=[N:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 818524-Chloropyridine hydrochlorideHCID 23438726HCID 23438726, Verbindung

Produkt 1

HCID 9888514HCID 9888514, VerbindungAusbeute 16,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A pressure tube (Aldrich) was charged with N-(5-chloropyridin-2-yl)-3-[(piperidin-4-ylmethyl)amino]pyridine-2-carboxamide (500 mg, 1.45 mmol), 4-chloropyridine hydrochloride (435 mg, 2.90 mmol), triethylamine (293 mg, 2.90 mmol) and EtOH (5 mL), sealed, and placed in a 110° C. bath. After 16 h, the mixture was cooled, concentrated, and the residue purified by column chromatography (SiO2: 5 to 7.5% methanol:methylene chloride) yielding 100 mg (16%) of the title compound.

Aufarbeitung

  1. customsealed
  2. customplaced in a 110° C.
  3. temperaturethe mixture was cooled
  4. concentrationconcentrated
  5. customthe residue purified by column chromatography (SiO2: 5 to 7.5% methanol:methylene chloride)

Quellen und Nachweise

ORD-Eintrag
ord-4774e93c69bc4d889f7300297b09f23c
Quelldatensatz
uspto-grants-2004_02
Patentnummer
US06689780B1

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