Réaction #47891

ord-1a283ebeecc94dc18563be03e16f73f1

Équation de réaction

COC=CC(=O)CC(=O)c1ccc(I)cc1
1-(4-iodo-phenyl)-5-methoxy-pent-4-ene-1,3-dione
COC=CC(=O)CC(=O)c1ccc(I)cc1
compound F1
COC=CC(=O)CC(=O)c1ccc(I)cc1
1-(4-iodo-phenyl)-5-methoxy-pent-4-ene-1,3-dione
NNC(N)=S
thiosemicarbazide
S=c1[nH]c(-c2ccc(I)cc2)cc2ccnn12
5-(4-Iodo-phenyl)-6H-pyrazolo[1,5-c]pyrimidine-7-thione

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températureis heated
  2. 2
    Températureto reflux temperature
  3. 3
    Filtrationis filtered
  4. 4
    Lavagewashed with methanol
  5. 5
    AutreThe filtrate with the product is purified by flash silica gel chromatography

Mode opératoire

A mixture of 1-(4-iodo-phenyl)-5-methoxy-pent-4-ene-1,3-dione (compound F1)(1.9 g) and thiosemicarbazide (5 g) in methanol (220 ml) is heated to reflux temperature. After the reaction is completed the solid is filtered and washed with methanol. The filtrate with the product is purified by flash silica gel chromatography.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07745446B2uspto-grants-2010_06