Synthetic method of royaljelly acid
A synthesis method and a royal jelly acid technology, applied in the field of medicine, can solve the problems of poor selectivity, difficult product purification, increased side reactions, etc., and achieve the effects of high stereoselectivity, serious environmental pollution, and improved stereoselectivity
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Examples
Embodiment 1
[0043] Preparation of 8-acetoxy-1-octanol (3)
[0044] 1,8-octanediol (10.00 g, FW: 146.22; 68.40 mmol) was dissolved in 100 ml of ethyl acetate, then 100 g of silica (100 mesh) was added to the solution, stirred, and then the solvent was concentrated Removed to obtain 1,8-octanediol adsorbed on silica.
[0045] At the same time, in a 1000mL three-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, the above-mentioned adsorbate, 500ml of cyclohexane, and acetyl chloride (6.44g, FW: 78.50; 82.10mmol) were added to the system in sequence. middle. The reaction temperature was then raised to 60° C., at which stirring was continued for 2 hours. After the completion of the reaction, the temperature of the system was cooled to room temperature, and then the mixture was filtered, and the filter cake was fully washed with ethyl acetate until there was no product in the filter cake. A colorless filtrate was obtained,...
Embodiment 2
[0047] Preparation of 8-acetoxy-1-octanol (3)
[0048] 1,8-octanediol (10 g, FW: 146.22; 68.40 mmol) was dissolved in 100 ml of ether, then 50 g of silicon dioxide (100 mesh) was added to the solution, stirred, and then the solvent was concentrated and removed to obtain 1,8-octanediol is adsorbed on silica.
[0049] At the same time, in a 1000mL three-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, the above-mentioned adsorbate, 500ml of petroleum ether, and acetyl chloride (10.74g, FW: 78.50; 136.81mmol) were sequentially added to the system . The reaction was then stirred for 12 hours at 20°C. After the completion of the reaction, the temperature of the system was cooled to room temperature, and then the mixture was filtered, and the filter cake was fully washed with ethyl acetate until there was no product in the filter cake. A colorless filtrate was obtained, the organic phases were combined and the...
Embodiment 3
[0051] Preparation of 8-propionyloxy-1-octanol (3)
[0052] 1,8-octanediol (10g, FW: 146.22; 68.40mmol) was dissolved in 100 ml of ether, then 100 g of silicon dioxide (100 mesh) was added to the solution, stirred, and then the solvent was concentrated and removed to obtain 1 , 8-octanediol is adsorbed on silica.
[0053] At the same time, in a 1000mL three-neck round-bottomed flask equipped with mechanical stirring, a thermometer, and a constant pressure dropping funnel, the above-mentioned adsorbate, 500ml of petroleum ether, and propionyl chloride (12.66g, FW: 92.52; 136.81mmol) were added to the system in sequence. middle. The reaction was then stirred for 4 hours at 60°C. After the completion of the reaction, the temperature of the system was cooled to room temperature, and then the mixture was filtered, and the filter cake was fully washed with ethyl acetate until there was no product in the filter cake. A colorless filtrate was obtained, the organic phases were combi...
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Application Information
- IPC
- C07C59/42; C07C51/377
- Inventors
- 严政军; 金燕华