Compound containing unsaturated double bond, oxygen absorber comprising same, and resin composition
An unsaturated, compound technology, used in organic chemistry, chemical instruments and methods, coatings, etc., can solve problems such as sticky surface and slow curing
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Embodiment 1
[0125] Synthesis of 1,3-bis(3-methyl-2-butenyloxy)-2-hydroxypropane
[0126] [chemical formula 9]
[0127]
[0128] Under a nitrogen stream, 61.8 g (0.717 mol) of 3-methyl-2-buten-1-ol and 36.84 g (0.657 mol) of potassium hydroxide were charged into a reactor equipped with a stirrer, a thermometer, and a dropping funnel. While keeping the internal temperature at 10° C. or lower, 19.34 g (0.209 mol) of epichlorohydrin was added dropwise while stirring, and the temperature was raised to 50° C. after the dropwise addition was completed. After stirring for 6 hours at an internal temperature of 50°C, it was cooled to 25°C. The reaction liquid was neutralized with a 4M aqueous hydrochloric acid solution, and the upper layer was washed with 310 mL of ion-exchanged water. The obtained organic layer was purified by distillation to obtain 28.77 g (0.126 mol; Yield 60.3%). The following shows its 1 Measurement results of H-NMR.
[0129] 1 H-NMR (400MHz, CDCl 3 , TMS) δ: 5.34 (...
Embodiment 2
[0131] Synthesis of 1,3-bis(3-methyl-2-butenyloxy)-2-methacryloyloxypropane
[0132] [chemical formula 10]
[0133]
[0134] Under the air flow, 16.1 g of acetonitrile and 11.43 g of 1,3-bis(3-methyl-2-butenyloxy)-2-hydroxypropane (0.050 mol), triethylamine 8.41g (0.083mol). Keeping the internal temperature below 15°C, 6.30 g of methacryloyl chloride (0.060 mol, containing 2200 ppm of p-methoxyphenol as a polymerization inhibitor) was added dropwise while stirring, and the temperature was raised to 25°C after the dropwise addition was completed. Stir for 1.5 hours at an internal temperature of 25°C. 7.07 g of ion-exchanged water and 61 mg of p-dimethylaminopyridine were added to the reaction liquid, and stirred at 25° C. for 2 hours. After confirming the decomposition of methacrylic anhydride as a by-product, extraction was performed three times with ethyl acetate. The organic layer was washed with 2% by mass aqueous hydrochloric acid solution, 3% by mass sodium bicarbon...
Embodiment 3
[0137] 5.00 g (21.9 mmol) of 1,3-bis(3-methyl-2-butenyloxy)-2-hydroxypropane produced in Example 1 and cobalt(II) stearate were added to a glass sample bottle (Manufactured by Wako Pure Chemical Industries, Ltd.; purity 90% by mass) 34 mg (0.048 mmol; 0.11 mol relative to the vinyl group in 1,3-bis(3-methyl-2-butenyloxy)-2-hydroxypropane %), fully stirred to obtain oxygen absorbing agent. Table 1 shows the evaluation results.
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