Reaktion #54714

Reaktionsgleichung

1-(2,6-dibromophenyl)thiourea

→

2,6-dibromophenylisothiocyanate

Lösungsmittel

chlorobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA suspension of 101 g
2. 2
   Temperaturrefluxed 20 hours
3. 3
   Filtrationthe resulting solution was filtered
4. 4
   Sonstigeevaporated
5. 5
   SonstigeThe tan solid obtained
6. 6
   Sonstigewas triturated with boiling petroleum ether
7. 7
   Filtrationfiltered
8. 8
   TemperaturOn cooling
9. 9
   SonstigeA portion was recrystallized from ether-petroleum ether
10. 10
    Sonstigeto give the analytical sample, m.p. 65°-66°

Vorschrift

A suspension of 101 g. (0.326 mole) of 1-(2,6-dibromophenyl)thiourea in 1 l. of chlorobenzene was stirred and refluxed 20 hours, and the resulting solution was filtered and evaporated. The tan solid obtained was triturated with boiling petroleum ether and filtered. On cooling, the filtrate deposited 63.4 g. of yellow needles of 2,6-dibromophenylisothiocyanate, m.p. 63°-65°. A portion was recrystallized from ether-petroleum ether to give the analytical sample, m.p. 65°-66°.

Quelle