A kind of synthetic method of phenyltetrahydrofuran ether compound
A technology of phenyltetrahydrofuran ether and tetrahydrofuran ether, which is applied in the field of synthesis of phenyltetrahydrofuran ether compounds, can solve the problems of expensive catalyst, high cost of raw materials, and difficult preparation, and achieve mild reaction conditions, simple preparation process, and wide application prospects Effect
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Embodiment 1
[0023] A kind of preparation method of 4-acetyl phenyl tetrahydrofuran ether, synthetic route is as follows:
[0024]
[0025] Concrete synthetic steps are as follows:
[0026] Mix 100g of 4-acetylphenol, 2000mL of dichloromethane, 0.19g of PPTS and 77.2g of dihydrofuran, and heat up to reflux. After 0.5h of reaction, LC detects that the reaction of the raw materials is complete, and the reaction is stopped;
[0027] Add 2000mL of water to the reaction solution, wash twice and separate the organic phase, dry the organic phase with anhydrous magnesium sulfate and concentrate under reduced pressure to obtain 151.1g of a light yellow solid, which is 4-acetylphenyltetrahydrofuran ether. The yield 99.6%, LC content 98.6%.
Embodiment 2
[0029] A preparation method of 4-isopropenyl phenyl tetrahydrofuran ether, the synthetic route is as follows:
[0030]
[0031] Concrete synthetic steps are as follows:
[0032] Mix 100g of 4-isopropenylphenol, 1000mL of chloroform, 1.87g of PPTS, and 78.3g of dihydrofuran, cool down to 0°C, and react for 5 hours. LC detects that the reaction of the raw materials is complete, and the reaction is stopped;
[0033] Add 2000mL of water to the reaction solution, wash twice and then separate the organic phase, dry the organic phase with anhydrous magnesium sulfate and concentrate under reduced pressure to obtain 149.6g of light yellow transparent liquid, which is 4-isopropenylphenyltetrahydrofuran ether. Yield 98.3%, LC content 98.5%.
[0034] figure 1 For the infrared spectrogram of the 4-isopropenyl phenyl tetrahydrofuran ether prepared in embodiment 2, figure 1 It can be seen that the wave number is 3085cm -1 、1627cm -1 They are carbon-hydrogen bonds in C=C-H and C=C str...
Embodiment 3
[0037] A preparation method of 4-ethylphenyl tetrahydrofuran ether, the synthetic route is as follows:
[0038]
[0039] Concrete synthetic steps are as follows:
[0040] Mix 100g of 4-ethylphenol, 1000mL of tetrahydrofuran, 20.6g of PPTS, and 286.8g of dihydrofuran, and heat up to 30°C. After 10 hours of reaction, LC detects that the reaction of the raw materials is complete, and the reaction is stopped;
[0041] Add 2000mL of water to the reaction solution, wash twice, separate the organic phase, dry the organic phase with anhydrous magnesium sulfate, and concentrate under reduced pressure to obtain 155.1g of light yellow transparent liquid, which is 4-ethylphenyltetrahydrofuran ether. The yield is 98.6%, and the LC content is 98.3%.
[0042] It can be seen that the preparation process of the present invention is simple, the catalytic efficiency of pyridine 4-methylbenzenesulfonate is high, the reaction conditions are mild, and the yield of the prepared product is as hig...
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