تفاعل #42749
ord-808de5774aaf47ca9c8db9011397b39c
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةis heated
- 2درجة الحرارةunder reflux for 2 h
- 3غسيلThe resulting aqueous suspension is washed with ethyl acetate (2×100 ml)
- 4غسيلThe combined organic layers are washed with water (3×100 ml) and brine (100 ml)
- 5تجفيفdried (magnesium sulfate)
- 6ترشيحfiltered
- 7أخرىThe solvent is removed by evaporation in vacuo
- 8أخرىto afford a dark brown oil
- 9أخرىThis 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.