Reaktion #2487284

ord-1c9d2da34322497cb55088a39411c298

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was cooled
  2. 2
    workup.ADDITIONpoured
  3. 3
    Sonstigeonto crushed ice
  4. 4
    FiltrationThe mixture was filtered
  5. 5
    Sonstigethe solid collected
  6. 6
    Waschenwas washed with water
  7. 7
    SonstigeThe solid was dried in a vacuum oven at 50° C.

Vorschrift

A stirred solution of 7.81 g (39.1 mmol) of 6-ethyl-2-phenyl-4(3H)-pyrimidinone and 5.80 g (43.4 mmol) of N-chlorosuccinimide in 100 mL of glacial acetic acid was heated at 90° C. for 4 h. The mixture was cooled, poured onto crushed ice and allowed to stand until the ice had melted. The mixture was filtered and the solid collected was washed with water and a little ether. The solid was dried in a vacuum oven at 50° C. to afford 7.99 g of 5-chloro-6-ethyl-2-phenyl-4(3H)-pyrimidinone (an intermediate for compound 172) as a white solid. 1H-NMR (d6-DMSO) 1.30(3H,t), 2.8(2H,q), 7.6(3H,m), 8.2(2H.m).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05453414uspto-grants-1995_09