Potassium Carbonate → HCID 44478092, Verbindung

HRID 2387710Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2387710
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[N:18]=[C:17]([NH:19][C:20](=[O:22])[CH3:21])[CH:16]=[CH:15][CH:14]=1)(C)C>CO>[C:12]([C:13]1[N:18]=[C:17]([NH:19][C:20](=[O:22])[CH3:21])[CH:16]=[CH:15][CH:14]=1)#[CH:11]

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 44478150N-(6-(2-(Trimethylsilyl)ethynyl)-2-pyridinyl)acetamide

Produkt 1

HCID 44478092HCID 44478092, VerbindungAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Anhydrous potassium carbonate (110 mg, 0.8 mmoles) was added to a solution of N-(6-((trimethylsilyl)ethynyl)pyridine-2-yl)acetamide (1.86 g, 8 mmol) in 20 ml anhydrous methanol. The reaction mixture was stirred at room temperature for fifteen minutes then filtered. The filtrate was concentrated in vacuo. The crude product mixture was chromatographed on Silica Gel (230-400 Mesh) eluting with 2.5% MeOH/98% CH2Cl2 to yield A436.1 as an off-white solid. (770 mg, 60% yield). M+H+=218.20 1H NMR (400 MHz) MEOD δ 8.13 (m, 1H), 7.75 (m, 1H), 7.27 (m, 1H), 3.65 (s, 1H), 2.18 (s, 3H).

Aufarbeitung

  1. filtrationthen filtered
  2. concentrationThe filtrate was concentrated in vacuo
  3. customThe crude product mixture was chromatographed on Silica Gel (230-400 Mesh)
  4. washeluting with 2.5% MeOH/98% CH2Cl2
  5. customto yield A436.1 as an off-white solid

Quellen und Nachweise

ORD-Eintrag
ord-76538b7f26d04baf89807dc939ae0aa2
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08268855B2

Notizen zur Reaktion

Wird geladen…