Reaktion #501852

ord-957e6e3651fb4d928c6a2e4935368d59

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturby heating under argon
  2. 2
    Temperaturat reflux for 90 minutes
  3. 3
    Temperaturreflux temperature
  4. 4
    workup.ADDITIONwas added slowly with good agitation
  5. 5
    Temperaturat reflux for two hours
  6. 6
    Filtrationto filter when it
  7. 7
    SonstigeTherefore, the solvent was removed under reduced pressure at 90°-100° C
  8. 8
    SonstigeThe dried solid obtained

Vorschrift

Following the procedure of Example 1, 24.3 gm of magnesium metal chips were placed in a 3 necked 3 liter reactor with 0.25 g I2 crystals and 1500 ml of Isopar G solvent. A fraction of isoparaffinic hydrocarbons (Isopar G) having a boiling range of 157° to 176° C. The magnesium was iodine-activated by heating under argon and at reflux for 90 minutes. The activated magnesium metal slurry in Isopar G was then reacted with 104 ml of n-butyl chloride (lM) at the solvent reflux temperature. After two hours of reaction, 125 ml of 2-methyl-1-pentanol was added slowly with good agitation. The thick reaction slurry was agitated at reflux for two hours. Because of the viscous nature of the thick slurry, it was difficult to filter when it was hot. Therefore, the solvent was removed under reduced pressure at 90°-100° C. The dried solid obtained was not a powder, but sticky gray flakes. Dried product was analyzed and found to contain 15.21% Mg; 58.95%

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04792640uspto-grants-1988_12