Method of preparing alpha-asarone
A kind of asarone, a certain amount of technology, applied in the field of preparation of organic compounds, can solve the problems of increasing production costs, difficult to complete dehydration reaction, unsuitable for industrial production, etc., to reduce raw material costs, reduce production costs, and shorten the synthesis route Effect
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Embodiment 1
[0034] Take 15g (72mmol) of mixed alkenes to a 250ml round bottom flask, add 100ml of benzene, add the catalyst PdCl 2 (CH 3 EN) 2 372 mg (1.44 mmol), heated and refluxed and stirred for 8 hours, isomerization reached equilibrium, GC showed trans / cis=93.5 / 6.5, stopped the reaction, removed the solvent under reduced pressure, added 50 ml of anhydrous diethyl ether, stirred for 5 minutes, and filtered on silica gel powder , the solvent was removed under reduced pressure to obtain an oil, which was recrystallized from n-hexane to obtain 10.7 g of white crystals, with a yield of 71.3%, and a melting point of mp60-61°C. 1 H NMR (CDCl 3 ): δ1.88 (dd, 3H, J=1.8, 6.8Hz, -CH 3 ), 3.82 (s, 3H, -OCH 3 ), 3.86(s, 3H, -OCH 3 ), 3.88(s, 3H, -OCH 3 ), 6.09(q, 1H, J=6.8, 15.7Hz, =CH), 6.49(s, 1H, PhH), 6.65(d, 1H, -CH=, 15.7Hz), 6.94(s, 1H, PhH) .
Embodiment 2
[0036] Take 5g (24mmol) of mixed alkenes to a 100ml round bottom flask, add 25ml CH 2 Cl 2 , adding catalyst PdCl 2 (PhCN) 2 184mg (0.48mmol), stirred at room temperature for 24h, isomerization reached equilibrium, GC showed trans / cis=94.0 / 6.0, stopped the reaction, removed the solvent under reduced pressure, added 25ml of anhydrous ether, stirred for 5min, and filtered on silica gel powder , the solvent was removed under reduced pressure to obtain an oil, which was recrystallized from n-hexane to obtain 3.1 g of white crystals, with a yield of 62.0%, melting point mp60-61°C, 1 H NMR (CDCl 3 ): δ1.88 (dd, 3H, J=1.8, 6.8Hz, -CH 3 ), 3.82 (s, 3H, -OCH 3 ), 3.86(s, 3H, -OCH 3 ), 3.88(s, 3H, -OCH 3 ), 6.09(q, 1H, J=6.8, 15.7Hz, =CH), 6.49(s, 1H, PhH), 6.65(d, 1H, -CH=, 15.7Hz), 6.94(s, 1H, PhH) .
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