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Novel 2-(amino) ethyl methyl sulfone salt and preparation

A technology of ethyl methyl sulfone hydrochloride and ethyl methyl sulfone, which is applied in the field of preparing high-purity 2-ethyl methyl sulfone, and can solve the problems such as difficult purification of hydrochloride

Inactive Publication Date: 2011-03-23
上海泺安医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the preparation, we found that the hydrochloride was difficult to purify

Method used

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  • Novel 2-(amino) ethyl methyl sulfone salt and preparation
  • Novel 2-(amino) ethyl methyl sulfone salt and preparation
  • Novel 2-(amino) ethyl methyl sulfone salt and preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0017] 2-(Amino)ethylmethylsulfone hydrogen sulfate

[0018] Add 30 liters of ethanol in the 50 liter kettle, add 0.58 kilograms of sodium hydroxide, stir to dissolve. Cool down to 20°C, add 2.3 kg of 2-(amino)ethylmethylsulfone hydrochloride in batches, and stir for 0.5 hours. Filter, wash the filter cake with ethanol, and combine the washing liquid and the filtrate. Cool to about 10°C, add 1.4 kg of p-toluenesulfonic acid in batches, and a white solid precipitates out. Stir for 2 hours, filter, and wash with ethanol to obtain 2.6 kg of 2-(amino)ethylmethylsulfone hydrogensulfate.

[0019] 2-(Amino)ethylmethylsulfone Sulfate

[0020] Add 30 liters of ethanol in the 50 liter kettle, add 0.58 kilograms of sodium hydroxide, stir to dissolve. Cool down to 20°C, add 2.3 kg of 2-(amino)ethylmethylsulfone hydrochloride in batches, and stir for 0.5 hours. Filter, wash the filter cake with ethanol, and combine the washing liquid and the filtrate. Cool to about 10°C, add 0.7 kg o...

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Abstract

The invention relates to the preparation of 2-(amino) ethyl methyl sulfone hydrochloride from an important intermediate of an anti-tumor medicament. In the conventional synthesis method, hydrochloride is difficult to purify because the hydrochloride is obtained by selectively reducing a sulfonyl-containing cyano compound with diborane and salifying with hydrogen chloride. The 2-(amino) ethyl methyl sulfone salt of other inorganic acid radicals and organic acid radicals prepared by the invention has the characteristic of high solubility and is easy to purify compared with the hydrochloride.

Description

technical field [0001] The invention relates to a new salt of 2-(amino)ethyl methyl sulfone and its preparation, which is beneficial to the preparation of high-purity 2-(amino) ethyl methyl sulfone. Background technique [0002] 2-(Amino)ethylmethylsulfone is an important intermediate in the synthesis of some active ingredients of antitumor drugs. Bibliographical reports 2-(amino) ethyl methyl sulfone synthetic route is as follows: [0003] [0004] Prepare the hydrochloride. During the preparation, we found that the hydrochloride was difficult to purify. Contents of the invention [0005] The shortcoming that the 2-(amino) ethyl methyl sulfone hydrochloride prepared by above route is difficult to purify, the present invention has prepared 2-(amino) ethyl methyl sulfone carboxylate, phosphate, dihydrogen phosphate, phosphoric acid Hydrogen di-salt, sulfonate, sulfate, bisulfate, carbonate, bicarbonate, borate, etc. The structures of other hydrohalides except hydrochl...

Claims

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Application Information

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IPC IPC(8): C07C317/28C07C315/04
Inventor 何勇
Owner 上海泺安医药技术有限公司
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