Š�-elemen-5-azacycle ramification and its synthetic method
A five-membered nitrogen heterocycle and elemene technology, applied in the direction of organic chemistry, can solve the problems of poor water solubility, and achieve the effects of mild reaction conditions, easy control of reaction conditions, and simple synthesis methods
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Embodiment 1
[0025] Step 1, β-elemene reacts with hypochlorite in acetic acid to prepare the halogenated product intermediate
[0026] In a 100mo round bottom bottle equipped with an electromagnetic stirrer, add 10.2g β-elemene and 10ml glacial acetic acid, and control the reaction temperature at about 0-5°C. Add 40ml of sodium hypochlorite (containing 8.6% available chlorine) dropwise from a constant pressure dropping funnel under vigorous stirring, and pay attention to maintaining the temperature of the reaction system not exceeding 5°C, and complete the addition within 4 hours. Stirring was continued at this temperature for 1 hour, then the reaction mixture was poured into a separatory funnel, extracted 3 times with petroleum ether (3×60 ml), and the organic phases were combined and dried over anhydrous sodium sulfate. The organic phase was concentrated to obtain a yellow oil, which was subjected to silica gel column chromatography to obtain 6.8 g of β-elemene chloride for the reaction ...
Embodiment 2
[0030] Step 1. FeCl 3 Treatment of other transition metals
[0031] Dissolve 5g of ferric chloride in 10mL of acetone, then add 20g of silica gel, remove acetone under reduced pressure on a rotary evaporator, then place the silica gel in an oven, dry at 120°C for 3-4 hours, and cool Store in a desiccator for later use. NiCl was prepared in the same way 2 , CoCl 2 catalyst. IrCl 3 The preparation method is to IrCl 3 Dissolve in 20ml of water, then distill off most of the water under reduced pressure, place the obtained powder in an oven, dry at 140°C for 4-5 hours, cool naturally and place in a desiccator for later use.
[0032] Step 2, β-elemene uses hypochlorite to prepare halogenated intermediates under the catalyzed reaction of transition metal chlorides
[0033] In a 100ml round bottom bottle equipped with an electromagnetic stirrer, add 10.2g β-elemene, 50ml n-hexane, FeCl 3 50%moL), cooled to below 0°C, and 40ml of sodium hypochlorite (containing 8.6% of availabl...
Embodiment 3
[0037] Step 1. FeCl 3 The processing such as transition metal is the same as embodiment 2.
[0038] Step 2, β-elemene uses NBS to prepare β-elemene bromide intermediate under transition metal chloride catalyzed reaction
[0039] In a 100mL round bottom bottle equipped with an electromagnetic stirrer, add 10.2g β-elemene, 30mL ether, 10% moL of cobalt dichloride, cool to below 0°C, add 10gNBS in batches under vigorous stirring, and react After 4 hours, the reaction solution was filtered, washed with n-hexane, and then the organic phase was concentrated and subjected to fast silica gel column chromatography, using petroleum ether as the eluent to remove inorganic salts and succinimide generated by the reaction to obtain unreacted β-elemene and β-elemene bromide, this mixture was used directly in the reaction of step 3. It is also possible to obtain a relatively pure β-elemene bromide for the reaction of step 3 by further column chromatography.
[0040] Step 3, preparation of ...
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