Reaktion #452489

ord-dcbdf60b2c55426b8ef6c9a1bbc4115d

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water
  2. 2
    Trocknendried over magnesium sulfate
  3. 3
    SonstigeAfter the resulting solution was purified
  4. 4
    Sonstigeon a silica gel column (developer: chloroform/methanol=40/1), recrystallization

Vorschrift

A mixture consisting of 7-(3-chloropropoxy)-2,3,4,5-tetrahydro-1H-benzoazepin-2-one (0.304 g, 1.2 mmol) and 1-(2-quinolylmethyl)piperazine (1.091 g, 4.8 mmol) was stirred for 4 hours at a bath temperature of 150° C. under an argon gas stream. The reaction mixture was dissolved in chloroform. The thus-obtained solution was rendered basic with a dilute aqueous solution of sodium hydroxide, washed with water, and then dried over magnesium sulfate. After the resulting solution was purified by subjecting it to chromatography on a silica gel column (developer: chloroform/methanol=40/1), recrystallization was conducted from acetone. The title compound (0.270 g) was obtained as yellow prisms (yield: 50.6%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06127360uspto-grants-2000_10