A method for synthesizing secondary alcohols in aqueous phase
A water-soluble, water-soluble technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve problems such as high reaction temperature and environmental pollution, achieve high yield, high conversion rate, and mild conditions
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Embodiment 1
[0032] Synthesize 1-phenylethanol 1-Phenylethanol, the structural formula is as follows:
[0033]
[0034] The method is: acetophenone (120 mg, 1.0 mmol), metal iridium complex [Cp*Ir(2,2'-bpyO)(OH)][Na] (4.6 mg , 0.01 mmol, 1 mol%) and water (1 mL) were successively added to a 25 mL round-bottomed flask, and the air in the round-bottomed flask was replaced with hydrogen, and the pressure of hydrogen in the system was maintained at 1 standard atmosphere throughout the reaction, and the reaction mixture was React at 30°C in a hydrogen atmosphere for 8 hours, 12 hours, and 16 hours, respectively. After the reaction, the solvent was removed by rotary evaporation, and then the pure target compound was obtained by column chromatography (developing solvent: petroleum ether / ethyl acetate volume ratio=8:1). In terms of acetophenone, calculate the product yield: 95%
[0035] The NMR spectrum of the obtained product is as figure 2 As shown, the NMR information is as follows:
[...
Embodiment 2
[0040] Synthesis of 1-phenylethanol 1-Phenylethanol, the method is: acetophenone (120 mg, 1.0 mmol), metal iridium complex [Cp*Ir(2,2'-bpyO)(OH)][Na] ( 4.6 mg , 0.01 mmol, 1 mol%) and water (1 mL) were successively added into a 25 mL round bottom flask, and the air in the round bottom flask was replaced with hydrogen, and the hydrogen in the system was maintained during the whole process of the reaction. The pressure was 1 standard atmosphere, and the reaction mixture was reacted at 15° C. in a hydrogen atmosphere for 18 hours. After the reaction, the solvent was removed by rotary evaporation, and then the pure target compound was obtained by column chromatography (developing solvent: petroleum ether / ethyl acetate volume ratio=8:1), with a yield of 94%.
Embodiment 3
[0042] Synthesis of 1-phenylethanol 1-Phenylethanol, the method is: acetophenone (120 mg, 1.0 mmol), metal iridium complex [Cp*Ir(2,2'-bpyO)(OH)][Na] ( 4.6 mg , 0.01 mmol, 1 mol%) and water (1 mL) were successively added into a 25 mL round bottom flask, and the air in the round bottom flask was replaced with hydrogen, and the hydrogen in the system was maintained during the whole process of the reaction. The pressure was 1 standard atmosphere, and the reaction mixture was reacted at 45° C. in a hydrogen atmosphere for 12 hours. After the reaction was completed, the solvent was removed by rotary evaporation, and then the pure target compound was obtained by column chromatography (developing solvent: petroleum ether / ethyl acetate volume ratio=8:1), with a yield of 95%.
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