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Water → 3-(Methoxymethyl)pyridine

HRID 1005375
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1005375
[OH:1][CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1.[H-].[Na+].I[CH3:12].O>O1CCCC1>[CH3:12][O:1][CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 6328Methyl iodideHCID 75103-PyridinemethanolHCID 24758Sodium hydride

Produkt 1

HCID 3389263-(Methoxymethyl)pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 3-hydroxymethylpyridine (10 g, 92 mmol) in anhydrous tetrahydrofuran (200 ml), under an atmosphere of nitrogen, was treated with sodium hydride (4 g of a 55% oil dispersion, 92 mmol) in portions. After stirring for 15 minutes iodomethane (5.7 ml, 92 mmol) was added dropwise and the reaction mixture was stirred at ambient temperature for 2 hours. Water (20 ml) was added and the tetrahydrofuran evaporated. The residue was partitioned between water (50 ml) and dichloromethane (70 ml). The organic layer was separated, dried (sodium sulphate) then evaporated. The crude product was purified by column chromatography on silica using ethyl acetate. The title compound was obtained (11 g, 93%) as an oil, δH (250 MHz, CDCl3) 3.42 (3H, s), 4.48 (2H, s), 7.27-7.32 (1H, m), 7.66-7.71 (1H, m), 8.53-8.60 (2H, m).

Aufarbeitung

  1. additionwas added dropwise
  2. customthe tetrahydrofuran evaporated
  3. customThe residue was partitioned between water (50 ml) and dichloromethane (70 ml)
  4. customThe organic layer was separated
  5. dry with materialdried (sodium sulphate)
  6. customthen evaporated
  7. customThe crude product was purified by column chromatography on silica

Quellen und Nachweise

ORD-Eintrag
ord-851e06dd801c4fc3807b95b8707281b1
Quelldatensatz
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06054469

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