Preparation method of nitrogen monoxide donor-type dehydroabietic acid derivatives
A technology for dehydroabietic acid and nitric oxide, which is applied in the field of preparation of dehydroabietic acid derivatives, can solve problems such as dehydroabietic acid derivatives that have not yet been found, and achieves high cost performance, low production cost and simple process. Effect
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Embodiment 1
[0036] One, the synthesis of intermediate 2-nitrooxyethylamine
[0037] Add 40mL of acetic anhydride to a 250mL two-necked flask and cool to -10°C, slowly add 12mL of fuming HNO 3 , and then 5 mL of ethyl acetate (40 mL) of ethanolamine was added dropwise to the above solution, and the mixture was warmed to 0 °C and stirred for one hour. Then change to room temperature and stir for 12 hours. After filtration, a white solid was obtained, which was washed with petroleum ether and dried to obtain 9.9 g of 2-nitrooxyethylamine, with a yield of 71.6% and a melting point of 104-106°C.
[0038] 2. Extraction of dehydroabietic acid
[0039]Put 50.0g of finely ground disproportionated rosin in a 250mL beaker, add 125mL of 95% (V / V) ethanol, heat to dissolve, pour it into a 250mL three-neck flask, heat the water bath to 80°C, add dropwise 9.8mL of ethanolamine (to disproportionate rosin After the reaction, add 125mL of hot deionized water (70-80°C), and carefully extract with isoocta...
Embodiment 2
[0046] One, the synthesis of intermediate 2-nitrooxyethylamine
[0047] Add 45mL of acetic anhydride to a 250mL two-necked flask and cool to -10°C, slowly add 15mL of fuming HNO 3 , and then 8 mL of ethyl acetate (45 mL) of ethanolamine was added dropwise to the above solution, and the mixture was warmed to 0 °C and stirred for one hour. Then change to room temperature and stir for 14 hours. After filtering, a white solid was obtained, which was washed with petroleum ether and dried to obtain 16.1 g of 2-nitrooxyethylamine, with a yield of 73.2% and a melting point of 104-106°C.
[0048] 2. Extraction of dehydroabietic acid
[0049] Put 40.0g of finely ground disproportionated rosin in a 250mL beaker, add 125mL of 95% (V / V) ethanol, heat to dissolve, pour it into a 250mL three-neck flask, heat the water bath to 90°C, add dropwise 9.8mL of ethanolamine (to disproportionate rosin After the reaction, add 125mL of hot deionized water (70-80°C), and carefully extract with isooct...
Embodiment 3
[0056] 1. Synthesis of intermediate 2,2'-dinitrooxydiethylamine
[0057] Add 40mL of acetic anhydride to a 250mL two-necked flask and cool to -10°C, slowly add 9.9mL of fuming HNO 3 , and then 5 mL of diethanolamine was added dropwise to the above solution, stirred for 5 minutes, then 50 mL of ice-cold ethyl acetate was added, and the reaction was continued for 2 h. Add cyclohexane to dilute, and a white precipitate precipitates out, which is filtered, washed 3 times with cyclohexane, and dried to obtain 2,2'-dinitrooxydiethylamine. (7.6g, 44.7% yield) with a melting point of 115-117°C.
[0058] 2. Extraction of dehydroabietic acid
[0059] Put 50.0g of finely ground disproportionated rosin in a 250mL beaker, add 125mL of 95% (V / V) ethanol, heat to dissolve, pour it into a 250mL three-neck flask, heat the water bath to 80°C, add dropwise 9.8mL of ethanolamine (to disproportionate rosin After the reaction, add 125mL of hot deionized water (70-80°C), and carefully extract wit...
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