Method for synthesizing 10-P-nitrobenz-oxy-capric acid
A technology for the synthesis of nitrophenoxydecanoic acid, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems that the process parameters are not given, the synthesis method is not specifically described, etc., and achieve Inexpensive, low cost, and easy to operate
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[0013] The concrete steps of the synthetic method of 10-p-nitrophenoxydecanoic acid are as follows:
[0014] 1) Add 10-bromodecanoic acid / methanol containing 1M catalyst and 200mL~2000mL organic solvent / mole 10-bromodecanoic acid in a molar ratio of 1:2~5, the organic solvent used is 70: 30:1 (v / v) hexane / ether / acetic acid mixed solvent, reflux reaction at 45~65°C for 10~30h, after the reaction is completed, cool to room temperature, use 1 / 5~1 / 2 reaction liquid volume Adjust the pH to 7-8 with saturated sodium bicarbonate, then extract 2-3 times with ether of 1-2.5 times the volume of the reaction solution, then wash with 1 / 10-1 / 4 of the volume of the extract, and wash the extract with anhydrous sulfuric acid Dry over sodium, filter, and distill under reduced pressure to remove the organic solvent;
[0015] 2) Add 10-bromodecanoic acid methyl ester / sodium p-nitrophenolate and 3~12L dimethyl sulfoxide with a molar ratio of 1:1.1~1.5 into the reaction flask, turn on the stirrer...
Embodiment 1
[0020] 1) Synthesis of methyl 10-bromodecanoate
[0021] In a 100mL dry three-necked flask, add 15.863g (60mmol) of 10-bromodecanoic acid, 7.32mL (180mmol) of anhydrous methanol containing 1M sulfuric acid, and 18mL of a mixed solvent (hexane / ether / acetic acid is 70:30:1 (v / v)), reflux reaction at 62°C for 12h, after the reaction is completed, cool to room temperature, adjust the pH to 7.0 with 10mL saturated sodium bicarbonate, then extract with 25mL ether for 2-3 times, and wash the obtained solution twice with 10mL of water , the extract was dried with 12.7 g of anhydrous sodium sulfate, filtered, and the organic solvent was distilled off under reduced pressure to obtain 15.0 g of a brown-red oily liquid with a yield of 94.3%. The refractive index is 1.4640 (20°C).
[0022] 2) Synthesis of 10-pNCAMe
[0023] Add 4.5g (17mmol) of methyl 10-bromodecanoate directly into a three-necked flask containing 100mL of DMSO solution containing 2.98g (18.5mmol) of sodium p-nitrophenol...
Embodiment 2
[0027] 1) Synthesis of methyl 10-bromodecanoate
[0028] In a 250 mL dry three-necked flask, add 15.863 g (60 mmol) of 10-bromodecanoic acid, 12.20 mL (300 mmol) of anhydrous methanol containing 1M sulfuric acid, and 100 mL of a hexane solvent system (hexane: ether: acetic acid 70:30: 1), reflux reaction at 48°C for 30h, after the reaction is completed, cool to room temperature, adjust the pH to 8.0 with 30mL saturated sodium bicarbonate, then extract with 100mL ether for 2 to 3 times, and wash the obtained solution twice with 25mL water, the extract Dry with 40g of anhydrous sodium sulfate, filter, and distill off the organic solvent under reduced pressure to obtain a brown-red oily liquid. Yield 91.2%. The refractive index is 1.4640 (20°C).
[0029] 2) Synthesis of 10-pNCAMe
[0030] Add 4.5g (17mmol) of methyl 10-bromodecanoate directly into a three-necked flask containing 100mL of DMSO solution containing 2.98g (18.5mmol) of sodium p-nitrophenolate, turn on the stirrer,...
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