A kind of preparation method of p-aminobenzene-beta-hydroxyethyl sulfone sulfate
A technology of hydroxyethyl sulfone and p-aminobenzene, which is applied in the field of preparation of p-aminobenzene-β-hydroxyethyl sulfone sulfate, can solve the problems of product quality and yield gap, and achieve increased yield and product quality , to achieve the effect of cost control
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[0037] Specifically, the steps of the preparation method of the present invention are as follows:
[0038] After reducing p-nitrochlorobenzene, it reacts and condenses with chloroethanol, then after the acylation reaction, catalyzes oxidation, and finally esterifies to obtain p-aminobenzene-β-hydroxyethyl sulfone sulfate;
[0039] By increasing the steps of the acylation reaction, the intermediate product can be made more stable, thereby further improving the quality of the product.
[0040] Preferably, the method steps of the present invention are as follows:
[0041] (i) Add water in p-nitrochlorobenzene, preferably, the mass ratio of p-nitrochlorobenzene and water is 50:100~110, more preferably, the mass ratio of p-nitrochlorobenzene and water is 50: 110;
[0042] Then, heat up and stir, and preferably heat up to 101-102°C;
[0043] Then, drop sodium sulfide solution, preferably, the mass percent of sodium sulfide solution used is 20~25%; More preferably, the mass percen...
Embodiment 1
[0080] (i) Add 50g of p-nitrochlorobenzene in the reaction kettle, then add 110g of water, stir and heat up to 101-102°C, start to add 60g of sodium sulfide solution (22%) dropwise, and the dropping time is controlled at 2-3 hours , after the dropwise addition is completed, the temperature of the reaction solution is controlled at 104-105°C;
[0081] Continue the reaction for 10 hours, then change the reflux device to a distillation device, distill out the by-product (a small amount of p-chloroaniline) at 106-108°C until the distillate is colorless, cool the reaction liquid to 5°C and filter, and collect the filtrate;
[0082] (ii) Move the filtrate obtained in step (i) into a reactor, add 80 g of chloroethanol (40%) at room temperature (cooled in a water bath) and stir for 1 hour, slowly add 40 mL of 36% hydrochloric acid, and stir for another 1 hour, and the reaction ends;
[0083] Pour the reaction solution into a 1000mL separatory funnel and let it stand for layering to se...
Embodiment 2
[0088] Prepare p-aminobenzene-β-hydroxyethyl sulfone sulfate with reference to the method of Example 1, wherein, in the step (i) of Example 2, the amount of water is 80g.
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