Sodium Methoxide → HCID 23144869, Verbindung

HRID 1393065Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1393065
C[O-].[Na+].Br[CH2:5][C:6]1[C:7]([N+:16]([O-:18])=[O:17])=[C:8]([CH:13]=[CH:14][CH:15]=1)[C:9]([O:11][CH3:12])=[O:10].[O:19]1CCOC[CH2:20]1.Cl>CO>[CH3:20][O:19][CH2:5][C:6]1[C:7]([N+:16]([O-:18])=[O:17])=[C:8]([CH:13]=[CH:14][CH:15]=1)[C:9]([O:11][CH3:12])=[O:10]

Komponenten

5

Versuchsvorschrift

Methanol solution (4.7 mL) of sodium methoxide (197 mg) was added dropwise into the mixture of methyl 3-bromomethyl-2-nitrobenzoate (1 g) and methanol (7 mL) under heating and refluxing. Two minutes later, the mixture was cooled down with ice and 1.82 mL of 4M hydrogen chloride dioxane solution was added dropwise thereto. After removing the solvent, diethylether and water were added and the organic layer thereof was dried over sodium sulfate. After removing the solvent, the obtained residue was purified with silica gel column chromatography to obtain 621 mg of methyl 3-methoxymethyl-2-nitrobenzoate.

Aufarbeitung

  1. temperatureunder heating
  2. temperaturerefluxing
  3. additionwas added dropwise
  4. customAfter removing the solvent, diethylether and water
  5. additionwere added
  6. dry with materialthe organic layer thereof was dried over sodium sulfate
  7. customAfter removing the solvent
  8. customthe obtained residue was purified with silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-950fb1c4009f4becac0f69404b81060e
Quelldatensatz
uspto-grants-2008_03
Patentnummer
US07345049B2

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