تفاعل #41947

ord-2e6422c6666e4cd8adb388d13ca64956

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe resulting mixture was evaporated to dryness
  2. 2
    استخلاصthe residue extracted with dichloromethane (2×), 1 N NaOH (2×) and sat. NaCl (1×)
  3. 3
    أخرىThe crude product was purified by chromatography on silica gel in dichloromethane
  4. 4
    أخرىThe product was crystallized from dichloromethane/heptane by evaporation of dichloromethane

الإجراء التجريبي

(2-Amino-5-bromo-phenyl)-(4-chloro-phenyl)-methanone (compound of example A.2) (4 g, 12.9 mmol), methanesulfonylacetone (2.63 g, 19.3 mmol) and sodium tetrachloroaureate(III) dihydrate (0.26 g, 0.64 mmol) were heated at reflux in 2-propanol (50 ml) for 4 days. The resulting mixture was evaporated to dryness and the residue extracted with dichloromethane (2×), 1 N NaOH (2×) and sat. NaCl (1×). The crude product was purified by chromatography on silica gel in dichloromethane. The product was crystallized from dichloromethane/heptane by evaporation of dichloromethane. One obtained a light yellow solid (1 g, 19%). MS: m/z=410 (M).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728142B2uspto-grants-2010_06