Reaktion #1472086

ord-c496d4f8cdbc412bb8c7f1c9284491fe

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 5 hours
  3. 3
    FiltrationThe obtained mixture was filtered
  4. 4
    Sonstigeto remove insolubles
  5. 5
    TrocknenThe organic layer of the filtrate was dried over magnesium sulfate
  6. 6
    Einengenconcentrated under a reduced pressure
  7. 7
    Sonstigeto give a crystalline residue
  8. 8
    WaschenThis residue was washed with chloroform

Vorschrift

A mixture comprising 339 mg of 2-chloro-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline, 500 mg of 4-hydroxypiperidine and 20 ml of N,N-dimethylformamide was heated under reflux for 5 hours and poured into 50 ml of water, followed by the addition of 50 ml of ethyl acetate. The obtained mixture was filtered to remove insolubles. The organic layer of the filtrate was dried over magnesium sulfate and concentrated under a reduced pressure to give a crystalline residue. This residue was washed with chloroform to give 145 mg of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06262059B1uspto-grants-2001_07