Synthesis method of spiro[2.5]octane-5-carboxylic acid
A synthesis method and technology of octane, applied in the direction of organic chemistry, nitrile preparation, etc., can solve the problems of expensive raw materials, inconvenient reaction operation, etc., and achieve the effect of saving synthesis cost and reasonable reaction process design
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Embodiment 1
[0012] Synthesis of 3-methoxy-cyclohexenone
[0013]
[0014] 100 g of 1,3-cyclohexanedione was added to 500 ml of methanol solution, 5 ml of concentrated sulfuric acid was added at room temperature, and the reaction temperature was raised to 65°C and stirred for 6 hours. After the reaction, the system was cooled to room temperature, 7.5 grams of sodium hydroxide was added to adjust the pH value of the system to 7, the solvent was evaporated to dryness under reduced pressure, extracted with tertiary methyl ether and water, the organic layer was dried by adding anhydrous sodium sulfate, filtered, and reduced The yellow oil was obtained by rotary steaming, the yield: 82%.
[0015] 1 H-NMR (CDCl3): 5.35 (s, 1H), 3.66 (s, 3H), 2.39-2.30 (m, 4H), 1.98-1.92 (m, 2H).
[0016] Synthesis of Methoxyspiro[2.5]oct-4-ene
[0017]
[0018] 48 g compound 2 Dissolve in 500 ml of toluene solution, add 195 g of isopropyl titanate at room temperature, stir for several minutes, add ...
Embodiment 2
[0020] Synthesis of 5-methoxyspiro[2.5]oct-4-ene
[0021]
[0022] 48 g compound 2 Dissolve in 500 ml of isopropyl ether solution, add 195 g of isopropyl titanate at room temperature, stir for several minutes, add 600 ml of ethyl Grignard reagent dropwise, and stir at room temperature for 3 hours. After the reaction was completed, saturated ammonium chloride solution was added to quench the reaction, the insoluble matter was filtered off, extracted with tertiary methyl ether, the organic layer was dried by adding anhydrous sodium sulfate, filtered, and rotary evaporated under reduced pressure to obtain a yellow oil, and the crude product was obtained. : 92%.
Embodiment 3
[0024] Synthesis of 5-methoxyspiro[2.5]oct-4-ene
[0025]
[0026] 48 g compound 2 Dissolve in 500 ml of tetrahydrofuran solution, add 195 g of isopropyl titanate at room temperature, stir for several minutes, add 600 ml of ethyl Grignard reagent dropwise, and stir at room temperature for 3 hours. After the reaction was completed, saturated ammonium chloride solution was added to quench the reaction, the insoluble matter was filtered off, extracted with tertiary methyl ether, the organic layer was dried by adding anhydrous sodium sulfate, filtered, and rotary evaporated under reduced pressure to obtain a yellow oil, and the crude product was obtained. : 30%.
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