A kind of synthetic method of thermosensitive chromogenic agent 4,4'-sulfonylbis[2-(2-propenyl)]phenol
A technology for the synthesis of sulfonyl bis, which is applied in the field of synthesis of heat-sensitive chromogenic agents, can solve the problems of large equipment investment, many side reactions, and high prices, and achieve the goal of reducing safety accidents, production costs, and equipment investment Effect
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Embodiment 1
[0033] Example 1 The synthetic method of 4,4'-sulfonyl bis[2-(2-propenyl)]phenol
[0034] Add 4,4'-diallyloxydiphenyl sulfone (33.0 g, 0.10 mol) and zinc chloride (0.33 g) into dichloromethane (100 mL), heat to 40°C and stir for 20 hours. After the reaction is complete, Cool down to room temperature and pour into 100mL 10%NaOH solution, stir to dissolve, then use 30%H 2 SO 4 Adjust the pH to about 9, continue to stir for 15 minutes, let stand and separate, recover the organic phase and use it mechanically, continue to adjust the pH to about 6 in the water phase at room temperature, filter, and dry to obtain 30g of white solid with a yield of 90.9% and a purity of 97%. .
[0035] The organic phase was recycled according to the above reaction conditions. After 10 times of recycling, the overall yield was 96%, and the purity was 96.5%.
[0036] ESI-MS: (m / z, %)=331(M+).
[0037] 1 H NMR (DMSO- d 6 ): δ=3.28(d, 4H, J = 8), 5.02 (d, 4H, J = 12), 5.85 (m, 2H), 6.90 (d, 2H...
Embodiment 2
[0038] Example 2 The synthetic method of 4,4'-sulfonyl bis[2-(2-propenyl)]phenol
[0039] Add 4,4'-diallyloxydiphenyl sulfone (33.0 g, 0.10 mol) and aluminum trichloride (0.66 g) into dichloromethane (100 mL), heat to 40°C and stir for 20 hours, the reaction is complete , pour it into 100mL 10%NaOH solution at room temperature, stir to dissolve, then use 30%H 2 SO 4 Adjust the pH to about 9, continue to stir for 15 minutes, let stand and separate, recover the organic phase and use it mechanically, continue to adjust the pH to about 6 in the water phase at room temperature, filter, and dry to obtain 28g of white solid, with a yield of 84.8% and a purity of 97.5%. .
[0040] The organic phase was recovered and applied mechanically according to the above reaction conditions. After 10 times of recovery and applied mechanically, the comprehensive yield was 94%, and the purity was 97%.
[0041] 1 H NMR and MS are consistent with Example 1.
Embodiment 3
[0042] Example 3 The synthetic method of 4,4'-sulfonyl bis[2-(2-propenyl)]phenol
[0043] Add 4,4'-diallyloxydiphenylsulfone (33.0 g, 0.10 mol) and ferric chloride (1.5 g) into 1,2-dichloroethane (100 mL), heat to 60°C and stir to react After 15 hours, the reaction was completed, lowered to room temperature and poured into 100mL 10%NaOH solution, stirred and dissolved, then washed with 30%H 2 SO 4 Adjust the pH to about 9, continue to stir for 15 minutes, let stand and separate, recover the organic phase and use it mechanically, continue to adjust the pH to about 6 in the water phase at room temperature, filter, and dry to obtain 31g of white solid, with a yield of 93.9% and a purity of 98%. .
[0044] The organic phase was recovered and applied mechanically according to the above reaction conditions. After 10 times of recovery and applied mechanically, the comprehensive yield was 98%, and the purity was 97.5%.
[0045] 1 H NMR and MS are consistent with Example 1.
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