Nitrogen → HCID 57960183, Verbindung

HRID 82843Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 82843
N#N.[OH:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([C:10]([O:12][CH3:13])=[O:11])[N:9]=1.[CH3:14]I>C(Cl)Cl>[CH3:14][O:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([C:10]([O:12][CH3:13])=[O:11])[N:9]=1

Komponenten

5

Edukt 3

HCID 947NitrogenHCID 6328Methyl iodideHCID 67281821Methyl 2-(hydroxymethyl)oxazole-4-carboxylate

Produkt 1

HCID 57960183HCID 57960183, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of methyl 2-(hydroxymethyl)oxazole-4-carboxylate (231 mg, 1.47 mmol) in CH2Cl2 (0.9 mL) was treated with MeI (0.11 mL, 1.76 mmol) followed by Ag2O (511 mg, 2.21 mmol) and the resulting mixture (protected from light) was stirred overnight at 40° C. The reaction mixture was filtered and the solvent was removed under reduced pressure. Purification of the residue by FC (1:1 hept-EA) gave the title compound as a colorless oil: TLC: rf (1:1 hept-EA)=0.33. LC-MS-conditions 07: tR=0.49 min, [M+H]+=172.20.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. customthe solvent was removed under reduced pressure
  3. customPurification of the residue by FC (1:1 hept-EA)

Quellen und Nachweise

ORD-Eintrag
ord-4bb216c17d44415d9ff82aa4f3b5dbd9
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846733B2

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