Synthesizing process of (S)-2-benzyloxy-pentan-3-one
A benzyloxypentyl, synthesis process technology, applied in the field of chemical synthesis, can solve problems such as not suitable for the preparation of kilogram-scale products, and achieve the effects of short time consumption, increased reaction temperature, and high safety performance
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Embodiment 1
[0026] Step (1). Add ethyl lactate (118g, 1mol) and tetrahydropyrrole (142g, 2mol) to a 1L three-necked reaction flask equipped with mechanical stirring, reflux condenser and thermometer, stir at room temperature for 30 minutes, and then heat to After refluxing for 24 hours, the temperature was lowered to 50° C., and excess tetrahydropyrrole and by-product ethanol were evaporated under reduced pressure to obtain 142 g of compound amide with a purity of 98%, which was directly used in the next reaction.
[0027] Step (2). Add the reaction product compound amide (1mol, 143g), potassium hydroxide (1.5mol), benzyl chloride (1.3mol) and 1000 ml of toluene to a 2L three-necked reaction flask equipped with mechanical stirring and a thermometer , stirred vigorously at 80-90°C for 10 hours, followed by GC analysis, and when the reaction reached the end point, add 200ml of water to separate the layers, extract the aqueous layer with 500ml of toluene, combine the organic layers, and wash ...
Embodiment 2
[0031] Step (1). Add (S)-2-hydroxypropionic acid ethyl ester (118g, 1mol) and tetrahydropyrrole (213g, 3mol) to a 1L three-necked reaction flask equipped with mechanical stirring, reflux condenser and thermometer, at room temperature Stir at low temperature for 30 minutes, then heat to reflux for about 12 hours, cool to 60°C, and evaporate excess tetrahydropyrrole and by-product ethanol under reduced pressure to obtain 143 g of crude product with a purity of 98%, which is directly used in the next reaction.
[0032]Step (2). Add compound amide (1mol, 143g), sodium hydroxide (3mol), benzyl chloride (1.3mol) and 1000ml of 2-methyltetrahydrofuran to a 2L three-necked reaction flask equipped with mechanical stirring and a thermometer, Stir vigorously at 60-80°C for 3 hours, follow-up analysis by GC, add 200ml of water to separate layers after the reaction reaches the end point, extract the aqueous layer with 500ml of 2-methyltetrahydrofuran, combine the organic layers, and wash wit...
Embodiment 3
[0036] Step (1). Add ethyl lactate (118g, 1mol) and tetrahydropyrrole (213g, 3mol) to a 1L three-necked reaction flask equipped with mechanical stirring, reflux condenser and thermometer, stir at room temperature for 30 minutes, and then heat to After refluxing for 16 hours, the temperature was lowered to 50°C, and excess tetrahydropyrrole and by-product ethanol were evaporated under reduced pressure to obtain 141 g of compound amide with a purity of 98.5%, which was directly used in the next reaction.
[0037] Step (2). Add the reaction product compound amide (1mol, 143g), sodium carbonate (3mol), benzyl chloride (1.5mol) and 1000ml of 2-methanol to a 2L three-necked reaction flask equipped with mechanical stirring and a thermometer 2-methyltetrahydrofuran, stirred vigorously at 60-75°C for 3 hours, followed by GC analysis. After the reaction reached the end point, 200ml of water was added to treat the layers, and the aqueous layer was extracted with 500ml of 2-methyltetrahydr...
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