تفاعل #1255061

ord-08e676161f9c467583948c19adbc1088

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONthe addition
  2. 2
    workup.WAITThe reaction is left
  3. 3
    workup.STIRRINGunder stirring for one night
  4. 4
    أخرىthe precipitate is separated by filtration
  5. 5
    أخرىdried under vacuum
  6. 6
    أخرىThe compound is crystallized by methanol

الإجراء التجريبي

A solution of KOH 50% (3 ml) is added to an equimolar solution of 7-(2-methylallyloxy)-8-acetyl-3-methylflavone (2.61 g, 0.0075 mol) and 3,4,5-trimethoxy-benzaldehyde (1.47 g, 0.0075 mol) in ethanol 95%; the addition is performed under energetic stirring at room temperature. The reaction is left under stirring for one night and then diluted with water and acidified; the precipitate is separated by filtration and dried under vacuum. The compound is crystallized by methanol to give 2.4 g of product m.p. 82-84° C., 1H-NMR (CDCl3) δ:1.76 (s, 3H); 2.20 (s, 3H); 3.82 (s, 3H); 4.62 (s, 2H); 5.05 (d, 2H, J=18 Hz); 6.95-7.10 (m, 3H); 7.09 (d, 1H); 7.10 (d, 1H, J=9 Hz); 7.31 (d, 1H, J=16 Hz); 7.40-7.45 (m, 3H); 7.55-7.58 (m, 2H); 7.31 (s, 2H); 8.32 (d, 1H, J=8.9 Hz).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06620842B2uspto-grants-2003_09