تفاعل #42749

ord-808de5774aaf47ca9c8db9011397b39c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةis heated
  2. 2
    درجة الحرارةunder reflux for 2 h
  3. 3
    غسيلThe resulting aqueous suspension is washed with ethyl acetate (2×100 ml)
  4. 4
    غسيلThe combined organic layers are washed with water (3×100 ml) and brine (100 ml)
  5. 5
    تجفيفdried (magnesium sulfate)
  6. 6
    ترشيحfiltered
  7. 7
    أخرىThe solvent is removed by evaporation in vacuo
  8. 8
    أخرىto afford a dark brown oil
  9. 9
    أخرىThis is purified by flash chromatography (hexane/ethyl acetate=1:1, followed by 100% ethyl acetate)

الإجراء التجريبي

A stirred mixture of 7-amino-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one (1.1 g, 3.35 mmol) and sodium formate (0.23 g, 3.35 mmol) in formic acid (50 ml) is heated under reflux for 2 h. After cooling to room temperature, the reaction mixture is poured into ice/water (300 ml) with stirring. The resulting aqueous suspension is washed with ethyl acetate (2×100 ml). The combined organic layers are washed with water (3×100 ml) and brine (100 ml), dried (magnesium sulfate) and filtered. The solvent is removed by evaporation in vacuo to afford a dark brown oil. This is purified by flash chromatography (hexane/ethyl acetate=1:1, followed by 100% ethyl acetate) to afford the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732435B2uspto-grants-2010_06