反应详情

温度

125 °C

A mixture of 2.44 g of compound of Example 6 and 12 mL of 70% sulphuric acid was stirred for 1.5 h at 125° C. The obtained reaction mixture was then cooled to room temperature, followed by careful pouring into 100 g of ice, dilution with water, alkalinization with 35% sodium hydroxide, and extraction with ethyl acetate (3×40 mL). The combined organic phases were then washed with water, dried on anhydrous sodium sulphate, and then evaporated to complete dryness under vacuum. The obtained crude was then purified by flash chromatography (ethyl acetate-2.2 N solution of ammonia in methanol 9.6:0.4). The recovered fractions were then evaporated to complete dryness, affording 1.87 g of the title product (82%).

1. customThe obtained reaction mixture
2. temperaturewas then cooled to room temperature
3. washThe combined organic phases were then washed with water
4. dry with materialdried on anhydrous sodium sulphate
5. customevaporated
6. customThe obtained crude
7. customwas then purified by flash chromatography (ethyl acetate-2.2 N solution of ammonia in methanol 9.6:0.4)
8. customThe recovered fractions were then evaporated