Reaktion #61360

ord-9152d2e5710b4945a499398c63afce63

Reaktionsgleichung

CNC(=S)NN
4-methyl-3-thiosemicarbazide
CC(C)=O
acetone
CC(=O)CCl
chloroacetone
CC(C)=NN=c1scc(C)n1C
3.4-Dimethyl-2(3H)thiazolone-(1-methylethylidene) hydrazone

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 2 hours
  2. 2
    Temperaturto reflux for 7 hours
  3. 3
    Einengenwas then concentrated
  4. 4
    SonstigeThe resulting crude product was recrystallized from acetone

Vorschrift

21 g (200 mmol) of 4-methyl-3-thiosemicarbazide in 1000 mL of acetone was heated at reflux for 2 hours. To this solution was then added dropwise 20.4 g (220 mmol) of chloroacetone. The reaction mixture was allowed to reflux for 7 hours and was then concentrated. The resulting crude product was recrystallized from acetone. This gave 23 g of an orange-colored powder (63% of the theoretical).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429274B2uspto-grants-2008_09