The synthetic method of para-ester
A synthesis method and para-ester technology, applied in the field of dye intermediates, can solve the problems of increased production costs and follow-up processing costs, and achieve the effects of stable product quality, mild reaction conditions, and easy-to-obtain reaction raw materials
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Embodiment 1
[0065] The synthetic method of the para-position ester that embodiment 1 provides, comprises the steps:
[0066] (a) Sulfonation reaction: After adding 20 mol of fuming sulfuric acid into the reaction tank, cool down to 12°C, add 5mol of chlorosulfonic acid, stir and react for 2 hours, add 10mol of acetanilide, control the reaction temperature to 15°C, and react 4 Hour;
[0067] (b) Chlorination reaction: warming up the reacted solution to 45° C., adding 14 mol of thionyl chloride, and adding carbon tetrachloride as an auxiliary agent, and reacting for 4 hours;
[0068] (c) Reduction reaction: add 10 mol of sodium sulfite, stir evenly, control the reaction temperature at 28° C., keep pH=7.5 with sodium hydroxide solution, and react for 2.5 hours to obtain a reduction reaction liquid;
[0069] (d) Condensation reaction: Add 15mol of ethylene oxide into the reduction reaction liquid, heat up to 60°C, and react for 4 hours;
[0070] (e) Hydrolysis and esterification reaction: a...
Embodiment 2
[0073] The synthetic method of the para-position ester that embodiment 2 provides, comprises the steps:
[0074] (a) Sulfonation reaction: After adding 15 mol of fuming sulfuric acid into the reaction tank, cool down to 15°C, add 5mol of chlorosulfonic acid, stir and react for 2 hours, add 10mol of acetanilide, control the reaction temperature to 15°C, and react 3 Hour;
[0075] (b) Chlorination reaction: warming up the reacted solution to 40° C., adding 12 mol of thionyl chloride, and adding carbon tetrachloride as an auxiliary agent, and reacting for 3 hours;
[0076] (c) Reduction reaction: add 11 mol of sodium sulfite, stir evenly, control the reaction temperature to 30° C., keep pH=7.5 with sodium hydroxide solution, and react for 2 hours to obtain a reduction reaction liquid;
[0077] (d) Condensation reaction: Add 15mol of ethylene oxide into the reduction reaction solution, heat up to 55°C, and react for 4 hours;
[0078] (e) Hydrolysis and esterification reaction: a...
Embodiment 3
[0081] The synthetic method of the para-position ester that embodiment 3 provides, comprises the steps:
[0082] (a) Sulfonation reaction: After adding 24 mol of oleum into the reaction tank, cool down to 12°C, add 6mol of chlorosulfonic acid, stir and react for 3 hours, add 10mol of acetanilide, control the reaction temperature to 20°C, and react 5 Hour;
[0083] (b) Chlorination reaction: the solution after the reaction is warmed up to 50°C, and 15mol of phosphorus pentachloride is added, and reacted for 5 hours;
[0084] (c) Reduction reaction: add 10 mol of sodium sulfite, stir evenly, control the reaction temperature to 30° C., keep pH=8.0 with sodium hydroxide solution, and react for 3 hours to obtain a reduction reaction solution;
[0085] (d) Condensation reaction: Add 13 mol of ethylene oxide into the reduction reaction solution, heat up to 65°C, and react for 5 hours;
[0086] (e) Hydrolysis and esterification reaction: add sulfuric acid to carry out esterification...
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