Reaktion #941529

ord-24aa06d178004867a09c8cf2f8c473d2

Reaktionsgleichung

Cc1ccncn1
4-methylpyrimidine
C=O
para-formaldehyde
OCCc1ccncn1
title compound
OCCc1ccncn1
4-(2-Hydroxyethyl)pyrimidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigesealed capacity pressure vessel at 165° C. for 3.5 hours
  2. 2
    TemperaturAfter cooling
  3. 3
    Sonstigethe solvents evaporated
  4. 4
    Sonstigeto afford an oil
  5. 5
    SonstigeThis was purified by silica column chromatography
  6. 6
    Wascheneluting with dichloromethane
  7. 7
    SonstigeThe ethyl acetate fractions were evaporated

Vorschrift

A mixture of 4-methylpyrimidine (10 g, 106 mmol) and para-formaldehyde (3 g) was stirred in a 50 mL sealed capacity pressure vessel at 165° C. for 3.5 hours. After cooling, ether was added and the solvents evaporated to afford an oil. This was purified by silica column chromatography using a Flashmaster system, eluting with dichloromethane, then chloroform, ether, and finally ethyl acetate. The ethyl acetate fractions were evaporated to afford the title compound as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07259163B2uspto-grants-2007_08