Triethylamine → HCID 67114669, Verbindung

HRID 77392

Reaktionsgleichung

Reaktionsgleichung von HRID 77392
Cl[C:2]1[CH:3]=[C:4]([C:9]([N+:12]([O-:14])=[O:13])=[CH:10][N:11]=1)[C:5]([O:7][CH3:8])=[O:6].[N:15]12[CH2:23][CH2:22][CH:19]([CH2:20][CH2:21]1)[NH:18][CH2:17][CH2:16]2.C(N(CC)CC)C>CO>[N:15]12[CH2:23][CH2:22][CH:19]([CH2:20][CH2:21]1)[N:18]([C:2]1[CH:3]=[C:4]([C:9]([N+:12]([O-:14])=[O:13])=[CH:10][N:11]=1)[C:5]([O:7][CH3:8])=[O:6])[CH2:17][CH2:16]2

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 3984071,4-Diazabicyclo(3.2.2)nonaneHCID 45480451Methyl 2-chloro-5-nitroisonicotinate2×

Produkt 1

HCID 67114669HCID 67114669, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of methyl 2-chloro-5-nitroisonicotinate (Intermediate 26A) (0.1 g, 0.46 mmol) in methanol (3 mL) under nitrogen was added 1,4-diazabicyclo[3.2.2]nonane (0.18 g, 0.55 mmol) and triethylamine (7 mg, 0.69 mmol), reaction then stirred overnight. The reaction mixture was concentrated and purified by a 10 g silica column eluting with 40% ethylacetate in hexane to afford methyl 2-(1,4-diazabicyclo[3.2.2]nonan-4-yl)-5-nitroisonicotinate.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. custompurified by a 10 g silica column
  3. washeluting with 40% ethylacetate in hexane

Quellen und Nachweise

ORD-Eintrag
ord-58bf59a0d92c41de8a1b2a730ea09187
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08841289B2

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