Method for compounding and purifying macamides
A technology for macamide and said macamide, which is applied in the field of synthesis and purification of macamide, can solve the problems of low maca content, complicated extraction and separation process, no chemical synthesis process preparation process, etc., and achieves simple steps and product purity. high effect
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Embodiment 1
[0032] In a glass bottle containing 300 mL of dichloromethane, add palmitic acid (1950 mg), EDC·HCL (1456.92 mg), HOBt·H 2 O (1030 mg) and triethylamine (2633.7 μL), their respective molar ratios were 1:1:1:2.5, and then stirred with a magnetic stirrer at room temperature for 20 h. Afterwards, benzylamine (830 μL) was added and reacted for 4 hours under the same conditions to obtain the final synthesis solution. After the above reaction solution was evaporated to dryness with a rotary evaporator, 10% HCL (100mL) and n-hexane (250mL) were added immediately, dissolved with ultrasonic assistance, and extracted to obtain a n-hexane layer; washed three times with 10% NaOH (50mL), and then Wash once with 10% HCL (50 mL), and finally transfer the n-hexane solution to a low-temperature environment at 4°C overnight; use a filter to obtain the precipitated crystals, and dry them to obtain the finished product.
[0033] Performance Testing:
Embodiment 2
[0041]In a glass bottle filled with 50 mL of dichloromethane, add linoleic acid (2363.32 μL), EDC·HCL (1457.41 mg), HOBt·H2O (1030 mg) and triethylamine (2633.7 μL) in their respective molar ratios of 1:1:1:2.5, then use a magnetic stirrer to stir at room temperature for 15 hours. Afterwards, benzylamine (830 μL) was added and reacted for 5 h under the same conditions to obtain the final synthesis solution. After the above reaction solution was evaporated to dryness with a rotary evaporator, 5% sulfuric acid (50mL) and n-hexane (50mL) were added immediately, dissolved with ultrasonic assistance, and extracted to obtain an acetone layer; washed three times with 10% CaOH (50mL), and then Wash once with 10% HCL (50mL), and finally transfer the n-hexane solution to a low-temperature environment of -10°C overnight; use a filter to obtain the precipitated crystals, and dry them to obtain the finished product.
[0042] Performance Testing:
Embodiment 3
[0050] In a glass bottle filled with 50 mL of dichloromethane, add linoleic acid (2363.32 μL), EDC·HCl (1457.41 mg), HOBt·H 2 O (103 mg) and triethylamine (2634 μL), their respective molar ratios were 1:1:1:2.5, and then stirred with a magnetic stirrer at room temperature for 10 h. Then m-methoxybenzylamine (984.31 μL) was added and reacted for 4 hours under the same conditions to obtain the final synthesis solution. After the above reaction solution was evaporated to dryness with a rotary evaporator, acetic acid (50mL) and diethyl ether (50mL) were added immediately, dissolved with ultrasonic assistance, and extracted to obtain a diethyl ether layer; washed three times with 10% KOH (50mL), and then washed with acetic acid (50mL ) was washed once, the ether solution was passed through a silica gel column, a mixed solution of petroleum ether and ethyl acetate silicon (1:1) was used as a solvent, and the solvent was evaporated to dryness to obtain a synthetic product.
[0051] ...
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