Adding a certain compound to certain chemical reactions, such as: 25392-41-0, 4-(Chloromethyl)-7-hydroxy-2H-chromen-2-one, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks
The crude product (2 g, 9.50 mmol) in 200 mL single neck flask, adding 1 n naoh (100ml) the concentrated solution immediately turned yellow, and the solution was placed in an oil bath and heated to reflux for 2 h, and after the reaction, cooling to room temperature, with concentrated sulfuric acid to adjust the pH to 2 -3, and the resulting solution with ethyl acetate (30 ml × 4) the extraction, combining the organic phase with saturated saline (20 ml × 2, washed, dried over anhydrous sodium sulfate, filtered Solvent, the filtrate is evaporated under reduced pressure to obtain gray-brown columnar crystalline 1.3 g, the crude yield 71.2% of the crude product (1 g, 5.20 mmol) suspended in 10 mL of methanol and added dropwise 0 5 Ml of concentrated sulfuric acid, after dropping, heating under reflux to react for about 4 h, after the reaction, the methanol was removed under reduced pressure, the residual liquid is poured into 30 ml of water, in ethyl acetate (20 ml × 3) extraction, combining the organic phase with saturated sodium bicarbonate solution (15 mL × 2) washing, saturated brine (15 mL × 2, washed, dried over anhydrous sodium sulfate, filtered, the filtrate is decompressed and evaporated to obtain an yellow-brown oil, column chromatography (petroleum ether/ethyl acetate, 80: 20 Purification, v/v) to obtain light yellow solid 0.75 g, 70% yield
At the same time, in my other blogs, there are other synthetic methods of this type of compound,25392-41-0, 4-(Chloromethyl)-7-hydroxy-2H-chromen-2-one, and friends who are interested can also refer to it.
Reference:
Patent; ChinaPharmaceutical University; Huang, Wenlong; QIAN, Hai; Li, Zheng; YANG, Jianyong; Su, Xin; Pan, MiaoBo; (22 pag.)CN105566267; (2016); A;,
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