Synthetic method of methyl cyclopentenolone
A technology of methyl cyclopentenol ketone and synthesis method, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc. higher question
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[0030] A synthetic method of methylcyclopentenolone, the method may further comprise the steps:
[0031] (1) Control reaction system at pH=2-7, preferably pH=3-6, temperature is 45-70 DEG C, under preferred 50-65 DEG C, monitor dimethylamine hydrochloride, formaldehyde aqueous solution and 2 with online infrared instrument -Methylfuran reaction generates N,N-dimethyl-5-methylfurfurylamine reaction process; wherein, the mol ratio of dimethylamine hydrochloride and formaldehyde is (1-1.2):1, preferably (1- 1.02):1; the mass concentration of formaldehyde aqueous solution is 37-40ωt%; the molar ratio of dimethylamine hydrochloride to 2-methylfuran is (1-1.3):1. Preferred (1.05-1.07):1.
[0032] When detecting the content of 2-methylfuran in the reaction solution<0.55%, then acidify the reaction system pH<1 with industrial hydrochloric acid with a concentration of 5-37ωt%, preferably 30ωt%, at 60-100°C, preferably 70-100°C, The time is 1-4h, preferably 2-3h to obtain the product ...
Embodiment 1
[0036] A synthetic method of methylcyclopentenolone, the method may further comprise the steps:
[0037] (1) Add 44.85g (0.55mol) dimethylamine hydrochloride and 19.59g (1.09mol) water into a 500ml four-neck flask, control the temperature to 50°C, add 42.08g (37-40%, 0.54mol) formaldehyde , adjust the pH of the reaction solution to 4.5, and start to add 42.69g (0.52mol) of 2-methylfuran dropwise after 0.5h of reaction;
[0038] Leverage React IR TM 15 Monitor the reaction solution and find that the content of 2-methylfuran is <0.55%, while the mass content of N,N-dimethyl-5-methylfurfurylamine is 46.24%. Then dilute hydrochloric acid is added to adjust the pH to 0.95, and the temperature is raised to 70 ℃, after 3 hours of reaction, adjust the pH to 12.5 with sodium hydroxide solution, and react at a temperature of 75-80℃ for 0.5 hours to obtain 2-(dimethylamino)-3-methyl-2-cyclopentene-1- The ketone content is 95.57%. After extraction, concentration and recovery of the sol...
Embodiment 2
[0042] A synthetic method of methylcyclopentenolone, the method may further comprise the steps:
[0043] (1) Add 44.85g (0.55mol) dimethylamine hydrochloride and 19.59g (1.09mol) water into a 500ml four-neck flask, control the temperature to 60°C, add 42.08g (37-40%, 0.54mol) formaldehyde , adjust the pH of the reaction solution to 4.5, and start to add 42.69g (0.52mol) of 2-methylfuran dropwise after 0.5h of reaction,
[0044] Leverage React IR TM 15 Monitor the reaction solution and find that the content of 2-methylfuran is <0.55%, while the content of N,N-dimethyl-5-methylfurfurylamine is 48.27%, then add dilute hydrochloric acid, adjust the pH to 0.95, and heat up to 80°C , after reacting for 3 hours, adjust the pH to 12.5 with sodium hydroxide solution, and react at a temperature of 75-80°C for 0.5 hours to obtain 2-(dimethylamino)-3-methyl-2-cyclopenten-1-one The content is 95.61%. After extraction, concentration and recovery of the solvent, 2.21g of the front fractio...
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