Reaktion #44926

ord-33c95e91bcc34572aa32018660fd2a43

Lösungsmittel

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is then refluxed for five hours
  2. 2
    FiltrationThe insoluble material is filtered off at 25° C
  3. 3
    WaschenThe filtrate is washed with water
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Sonstigethe solvents are evaporated off (orange-coloured oil: 19.7 g; 99%)

Vorschrift

A mixture of 14 g (74 mmol) of ethyl (E)-3-phenylbut-2-enoate, 0.47 g of 2,2′-azobis(2-methylpropionitrile) and 330 ml of carbon tetrachloride is heated to 75° C. 19.8 g (111 mmol) of N-bromosuccinimide are added portionwise at this temperature. The mixture is then refluxed for five hours. The insoluble material is filtered off at 25° C. The filtrate is washed with water and dried over Na2SO4; the solvents are evaporated off (orange-coloured oil: 19.7 g; 99%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737176B2uspto-grants-2010_06