New technology of synthesizing 4-[2-(cyclo propyl methoxy] ethyl] phenol
A technology of cyclopropylmethoxy and tert-butoxybenzene, applied in the field of preparing 4-[2-ethyl]phenol, which can solve the problems of long route, low yield and high price
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Embodiment 1
[0012] Embodiment 1: add 128.0 grams (1 mole) p-chlorophenol, 200 milliliters of toluene and a few drops of methanesulfonic acid in four-necked bottle, pass into isobutylene at 35 ℃, keep certain ventilation rate, ventilate at constant temperature for 10 After 1 hour, the amount of isobutene was controlled at 1.30 moles, reacted at 45° C. for another 15 hours, and weighed. Add a small amount of water, heat to drive off excess isobutylene, weigh after liquid separation, add alkali to wash twice to remove unreacted phenol, and weigh after washing. Then washed with water for 3-4 times, evaporated the solvent to obtain 153.0 g of crude product, and rectified under reduced pressure to obtain 141.0 g of p-chlorophenyl tert-butyl ether. The yield was 76.4%, and the content was 99.5% (GC).
[0013] IR(KBr): 2980, 1890, 1590, 1480, 1390, 1360, 1240, 1080, 1155, 1055, 890, 850 1 H-NMR (CDCl 3 / TMS): δ1.34 (9H, s), 6.90 (2H, d), 7.20 (2H, d)
Embodiment 2
[0014] Embodiment 2: Add 128.0 grams (1 mole) p-chlorophenol, 200 milliliters of chlorobenzene and a few drops of dilute sulfuric acid in a four-necked bottle, feed isobutylene at 15 ° C, keep a certain ventilation rate, and ventilate at a constant temperature for 10 After 1 hour, the amount of isobutene was controlled at 1.30 mol, reacted at 25° C. for another 15 hours, and weighed. All the other operations are the same as in Example 1, the yield of p-chlorophenyl tert-butyl ether is 68.8%, and the content is 99.5% (GC).
Embodiment 3
[0015] Example 3: Add 128.0 grams (1 mole) of p-chlorophenol, 200 milliliters of dichloromethane and a few drops of dilute sulfuric acid in a four-necked bottle, feed isobutylene at 25° C., keep a certain rate of ventilation, and ventilate at a constant temperature After 10 hours, the amount of isobutylene was controlled at 1.30 mol, and the reaction was carried out at 30° C. for another 15 hours, and the mixture was weighed. All the other operations are the same as in Example 1, the yield of p-chlorophenyl tert-butyl ether is 69.5%, and the content is 99.2% (GC).
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