Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 111-45-5, name is 2-(Allyloxy)ethanol. A new synthetic method of this compound is introduced below., Product Details of 111-45-5
In a one-liter flask equipped with a stirring device, a dimroth condenser, a thermometer and a dropping funnel, put were 38.25 g (0.375 mol) of ethylene glycol monoallyl ether represented by the following formula (7) and 100 g of toluene, and heated to 70 degrees C. 0.38 Gram of a solution of a catalyst, complex of alkali-neutralized chloroplatinic acid with vinyl siloxane, in toluene, containing 0.5% of platinum, was added in the flask. Then, 185 g (0.25 mol) of the compound represented by the aforesaid formula (6) was added dropwise in the flask with the dropping funnel over one hour. The reaction mixture was held at 100 degrees C. for one hour and, then, analyzed in GC. The peak of the compound represented by the aforesaid formula (6) disappeared, which means that the reaction completed. 100 Grams of ion exchanged water were added to the reaction mixture with stirring to wash it and, then, left standing to cause phase separation. The aqueous phase containing the excessive ethylene glycol monoallyl ether was removed. The organic phase was similarly washed twice with each 100 g of ion exchanged water and, then, the toluene in the organic phase was stripped off under a reduced pressure to obtain 193.7 g (0.23 mol) of a colorless and transparent liquid, silicone compound represented by the following formula (8). The yield was 92%. The ratio of the silicone compound represented by the following formula (8) in the obtained product was 98.1 mass %, as determined in GC. In a one-liter flask equipped with a stirring device, a dimroth condenser, a thermometer and a dropping funnel, put were 210.5 g (0.25 mol) of the silicone compound represented by the formula (8), 0.02 g (0.01 mass %) of dioctyl tin oxide, 0.01 g of Ionol, i.e. 2,6-di-tert-butyl-4-methylphenol, ex Japan Chemtech Co. Ltd., and 0.01 g of 4-methoxyphenol to prepare a mixture. 40.3 Grams (0.26 mol) of a methacryl group-containing isocyanate compound represented by the following formula (9) was added dropwise to the mixture over one hour. The internal temperature rose from 20 degrees C. up to 40 degrees C. The mixture was held at 40 degrees C., while monitoring the peak of the silicone compound represented by the formula (8) in GC. Four hours later, the intensity of the peak of the silicone compound fell down below the detection limit by GC and, then, 4.0 g (0.125 mol) of methanol was added to the reaction mixture. Further, 180 g of hexane and 180 g of ion exchanged water were added to the reaction mixture to wash it. The reaction mixture was left standing to cause phase separation. The aqueous phase was removed and, subsequently, the organic phase was washed twice with ion exchanged water. The solvent, hexane, was stripped off from the organic phase under a reduced pressure to obtain 204.3 g of a colorless and transparent liquid product. 1H-NMR analysis showed that the obtained compound in the product was a silicone compound represented by the following formula (10), hereinafter referred to as silicone compound 1. The yield was 82% and the aforesaid amount (204.3 g) was 0.20 mol. The ratio of the silicone compound represented by the following formula (10) in the product was 97.1 mass %, as determined in GC, the viscosity was 112.9 mm2/s at 25 degrees C., the specific gravity was 1.165 at 25 degrees C. and the refraction index was 1.4131.
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Reference:
Patent; SHIN-ETSU CHEMICAL CO., LTD.; KUDO, Muneo; ICHINOHE, Shoji; GOTO, Tomoyuki; US2015/361113; (2015); A1;,
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