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Method for preparing N,N-dihydroxypropyl p-toluidine

A technology of p-toluidine and dihydroxypropyl, which is applied in the field of organic compound preparation, can solve problems such as unfavorable economic benefits, long production time, and unclear end point, and achieve the effects of shortening reaction time, convenient operation, and simple and easy-to-obtain raw materials

Inactive Publication Date: 2018-03-20
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N, the usual production method of N-dihydroxypropyl-p-toluidine is to carry out aminolysis synthesis by p-chlorotoluene and N, N-dihydroxypropylamine, the problems that this kind of preparation method exists: 1, because this reaction proceeds Time is difficult to control, the reaction time is as long as nearly 100 hours, and the end point is not clear
2. The raw material N, N-dihydroxypropylamine is not easy to obtain, and the cost is extremely high. Therefore, the method has the problems of long production time and low production efficiency, and the cost is extremely high, which is not conducive to the improvement of economic benefits of enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This preparation N, the method for N-dihydroxypropyl p-toluidine comprises the following steps:

[0022] ⑴ Aminolysis reaction steps

[0023] Put 1000 grams of p-methylaniline, 2000 grams of sodium hydroxide, and 4100 grams of methanol into a 10-liter reactor with a heating device, electric stirring, and a thermometer, and heat to 55 ± 2 ° C while stirring. Temperature state, add compound aminolysis initiator 350 grams, constantly add 4150 grams of chloropropanols, after adding chloropropanols, heat preservation reaction for 2 hours. Heating was stopped, and the aminolysis reaction was terminated.

[0024] ⑵ Filtration steps

[0025] Cool the mixture obtained after the aminolysis reaction to room temperature, filter, and collect the filtrate—an oily liquid.

[0026] ⑶ Distillation steps

[0027] The oil layer is distilled to obtain N,N-dihydroxypropyl-p-toluidine with a content of more than 96.5%.

Embodiment 2

[0029] This preparation N, the method for N-dihydroxypropyl p-toluidine comprises the following steps:

[0030] ⑴ Aminolysis reaction steps

[0031] Put 1000 grams of p-methylaniline, 2000 grams of sodium hydroxide, and 4100 grams of methanol into a 10-liter reactor with a heating device, electric stirring, and a thermometer, and heat to 55 ± 2 ° C while stirring. Temperature state, add compound aminolysis initiator 380 grams, constantly add 4150 grams of chloropropanols, after adding chloropropanols, heat preservation reaction for 2 hours. Heating was stopped, and the aminolysis reaction was terminated.

[0032] ⑵ Filtration steps

[0033] Cool the mixture obtained after the aminolysis reaction to room temperature, filter, and collect the filtrate—an oily liquid.

[0034] ⑶ distillation steps

[0035] The oil layer is distilled to obtain N,N-dihydroxypropyl-p-toluidine with a content of more than 96.5%.

Embodiment 3

[0037] This preparation N, the method for N-dihydroxypropyl p-toluidine comprises the following steps:

[0038] ⑴ Aminolysis reaction steps

[0039] Put 1000 grams of p-methylaniline, 2000 grams of sodium hydroxide, and 4100 grams of methanol into a 10-liter reactor with a heating device, electric stirring, and a thermometer, and heat to 55 ± 2 ° C while stirring. Temperature state, add compound aminolysis initiator 400 grams, continuously add 4150 grams of chloropropanols, after adding chloropropanols, heat preservation reaction for 2 hours. Heating was stopped, and the aminolysis reaction was terminated.

[0040] ⑵ Filtration steps

[0041] Cool the mixture obtained after the aminolysis reaction to room temperature, filter, and collect the filtrate—an oily liquid.

[0042] ⑶ distillation steps

[0043] The oil layer is distilled to obtain N,N-dihydroxypropyl-p-toluidine with a content of more than 96.5%.

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Abstract

The invention relates to a method for preparing N,N-dihydroxypropyl-p-toluidine. The method comprises the following steps: (1) Aminolysis reaction step, putting p-toluidine, chloropropanol, sodium hydroxide, and methanol into a reaction kettle In, stirring, heating and adding compound aminolysis initiator to react; (2) Filtration step, filtering the mixture after the aminolysis reaction, and separating the filtrate-oily liquid; (3) Distillation step, distilling the separated filtrate-oily liquid mixture to obtain N,N‑Dihydroxypropyl-p-toluidine product. In the synthesis step of the N,N-dihydroxypropyl-p-toluidine preparation method, a direct aminolysis reaction is used, and the quality of the prepared product fully meets the technical index requirements. The preparation method shortens the reaction time during production, uses simple and easy-to-obtain raw materials, reduces production costs, and improves the market competitiveness of products.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective preparation method of N,N-dihydroxypropyl-p-toluidine. Background technique [0002] In the industrial production of chemical catalytic curing, N,N-dihydroxypropyl-p-toluidine, as an important organic compound, has catalytic curing properties and is more and more widely used. N, the usual production method of N-dihydroxypropyl-p-toluidine is to carry out aminolysis synthesis by p-chlorotoluene and N, N-dihydroxypropylamine, the problems that this kind of preparation method exists: 1, because this reaction proceeds Time is difficult to control, the reaction time is as long as nearly 100 hours, and the end point is not clear. 2. The raw material N, N-dihydroxypropylamine is difficult to obtain and the cost is extremely high. Therefore, the method has the problems of long production time and low production efficiency, and the cost is extremely high...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C215/16
CPCC07C213/02C07C213/10C07C215/16
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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