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Preparation method of methyl p-tolyl sulfone

A technology of p-methylsulfonyl and p-toluenesulfonyl chloride, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve problems such as poor market competitiveness, long production cycle, and poor product quality, and achieve product The effect of good quality, low production cost and reduced production cost

Inactive Publication Date: 2010-03-03
SHANDONG XINGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The technical defect is that dimethyl sulfate highly toxic chemicals are used as raw materials, which is dangerous during operation and pollutes the environment; the production cycle is long, the product quality is poor, and the yield is low; resulting in high production costs and poor market competitiveness

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Using p-toluenesulfonyl chloride, anhydrous sodium sulfite, sodium bicarbonate, and methylene chloride as synthetic raw materials; including the following steps:

[0049] a. p-toluenesulfonyl chloride salt:

[0050]In a 2000L reactor, add 1400 kg of water, 260 kg of anhydrous sodium sulfite, and 300 kg of sodium bicarbonate; under stirring, raise the temperature to 40°C and stop heating; Add 350 kg of p-toluenesulfonyl chloride, control the temperature between 40°C-64°C, and complete the addition in about 1.5-2.5 hours; keep the reaction at 64°C for 1.5 hours, and complete the following reaction:

[0051] Na 2 SO 3 +2NaHCO 3 +C 7 h 7 ClO 2 S

[0052] →2CO 2 +H 2 O+NaCl+Na 2 SO 4 +C 7 h 7 NaO 2 S;

[0053] Put in 15 kg of activated carbon, keep warm and decolorize for 50-60 minutes, and circulate and filter while it is hot. After the circulating mother liquor is clear and transparent, enter the methylation reaction kettle for standby;

[0054] ...

Embodiment 2-9

[0064] According to the formula and steps of Example 1, the p-thiamphenicol toluene of the present invention was prepared according to the methylation-related process indicators in Table 1.

[0065] Table 1

[0066] project

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PUM

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Abstract

The invention relates to a preparation method of methyl p-tolyl sulfone, which belongs to the technical field of sulphone preparation, in particular to a preparation method of the methyl p-tolyl sulfone by taking monochloro methane as a methylating agent for synthesis. The preparation method is characterized by taking p-toluenesulfonylchloride, anhydrous sodium sulfite, sodium bicarbonate and monochloro methane as synthesizing raw materials and comprising the following operation steps: a. salifying the p-toluenesulfonylchloride; b. synthesizing the methyl p-tolyl sulfone; c. adjusting pH, reducing the temperature and discharging; d. filtering, dehydrating and drying; and e. inspecting the quality and packaging and warehousing after qualification. The invention provides a preparation methodof the methyl p-tolyl sulfone without using a deadly poisonous compound of dimethyl sulfate as a raw material, and has safe operation, environmental protection, short production period, good productquality, high yield, low production cost and strong market competitiveness. The content of the methyl p-tolyl sulfone reaches up to 99.5 percent, and the yield of the methyl p-tolyl sulfone, which iscounted by the p-toluenesulfonylchloride of the raw material, is more than or equal to 85 percent.

Description

technical field [0001] The invention is a preparation method of p-thiamphenicol toluene. The invention belongs to the technical field of preparation of sulfone. In particular, it relates to a preparation method for synthesizing p-thiamphenicol toluene with chloromethane as a methylating agent. Background technique [0002] P-thiamphenicol is an important starting material for the synthesis of medicines, dyes, and pesticides. Such as methafenmycin, fluprofen and so on. In the prior art, p-toluenesulfonyl chloride is used, reduced by sodium sulfite under weakly alkaline conditions, and then methylated with dimethyl sulfate or sodium methyl sulfate to synthesize p-thiamphenyl toluene. The technical defect is that dimethyl sulfate highly toxic chemicals are used as raw materials, which is dangerous during operation and pollutes the environment; the production cycle is long, the product quality is poor, and the yield is low; resulting in high production costs and poor market c...

Claims

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Application Information

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IPC IPC(8): C07C317/14C07C315/00
Inventor 高庆辉侯诗东韩己强
Owner SHANDONG XINGHUI CHEM
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