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A method for reclaiming 3-ethoxyl-4-methoxyl-alpha-[(methylsulfonyl)methyl]-benzylamine

A methylsulfonyl, methoxyphenyl technology, applied in the preparation of carboxylic acid amides, organic chemistry methods, chemical instruments and methods, etc., can solve problems such as unavailability, achieve prevention of solid waste, reduce environmental pollution, The effect of reducing production costs

Active Publication Date: 2021-06-15
SHANDONG ZOUPING DAZHAN NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the compound that cannot utilize another configuration of 3-ethoxyl-4-methoxyl-alpha-[(methylsulfonyl)methyl]-benzylamine in the prior art, the present invention provides a kind of recovery 3 - Ethoxy-4-methoxy-α-[(methylsulfonyl)methyl]-benzylamine method to solve the above problems

Method used

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  • A method for reclaiming 3-ethoxyl-4-methoxyl-alpha-[(methylsulfonyl)methyl]-benzylamine
  • A method for reclaiming 3-ethoxyl-4-methoxyl-alpha-[(methylsulfonyl)methyl]-benzylamine
  • A method for reclaiming 3-ethoxyl-4-methoxyl-alpha-[(methylsulfonyl)methyl]-benzylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) Synthesis of Compound II and Compound III

[0037] Based on the weight of Compound I, weigh 100g of Compound I, add 600g of purified water and 9.5g of sodium hydroxide, heat up to 40-80°C, keep warm for 2h, cool down to 10-30°C, and filter to obtain a filter cake and filtrate. Filter cake is compound II wet product, stand-by;

[0038] Add hydrochloric acid to the filtrate to adjust the pH to 2-3, stir at 20-30°C for 1 h, and filter with suction to obtain the wet product of Compound III. The compound III wet product was rinsed with water, the washing liquid was combined into the filtrate, and the compound III wet product was dried to obtain 32.5 g of compound III, with a yield of 83.8%.

[0039] (2) Synthesis of compound IV

[0040] Under stirring, add solid sodium bicarbonate to the filtrate obtained in step (1), adjust the pH of the reaction solution to 7-8, add the wet product of compound II prepared in step (1), heat up to 90-100°C, and keep stirring for 40 hou...

Embodiment 2

[0052] (1) Synthesis of Compound II and Compound III

[0053]Based on the weight of Compound I, weigh 500kg of Compound I, add 3000kg of purified water and 47.5kg of sodium hydroxide, heat up to 40-80°C, keep warm for 2h, cool down to 10-30°C, and filter to obtain a filter cake and filtrate. Filter cake is compound II wet product, stand-by;

[0054] Add hydrochloric acid to the filtrate to adjust the pH to 2-3, stir at 20-30°C for 1 hour, and filter with suction to obtain a wet product of the compound. The wet product of the compound was rinsed with water, the washing liquid was combined into the filtrate, and the wet product of the compound was dried to obtain 150 kg of compound III, with a yield of 77.4%.

[0055] (2) Synthesis of compound IV

[0056] Under stirring, add solid sodium bicarbonate to the filtrate obtained in step (1), adjust the pH of the reaction solution to 7-8, add the wet product of compound II prepared in step (1), heat up to 90-100°C, and keep stirring...

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Abstract

The invention relates to a method for recovering 3-ethoxy-4-methoxy-α-[(methylsulfonyl)methyl]-benzylamine, which belongs to the technical field of chemical synthesis. The technical scheme of the present invention is as follows: first, compound I, a by-product of the product, is free to recover compound III, and intermediate II is subjected to deamination reaction to generate intermediate IV, and then intermediate IV is subjected to an addition reaction to generate compound V. The beneficial effects of the present invention are: (1) the synthetic method of the present invention successfully recycles the by-products after splitting, preventing the generation of solid waste and reducing environmental pollution; (2) the synthetic method of the present invention The by-products after dismantling were successfully recycled and reused, which reduced the production cost from the original 1504 yuan / kg to 1002.67 yuan / kg. After continuous production, the cost will continue to be reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for recovering 3-ethoxy-4-methoxy-α-[(methylsulfonyl)methyl]-benzylamine. Background technique [0002] (S)-1-(3-Ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethylamine-N-acetyl-L-leucine salt is a synthetic apremilast important intermediates. The synthesis of (S)-1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethylamine-N-acetyl-L-leucine salt is mainly through the 3 -Ethoxy-4-methoxy-α-[(methylsulfonyl)methyl]-benzylamine was obtained by resolution. After splitting, the remaining compound in another configuration loses its use value and cannot be recycled, which causes waste of resources and increases production costs. Contents of the invention [0003] Aiming at the compound that cannot utilize another configuration of 3-ethoxyl-4-methoxyl-alpha-[(methylsulfonyl)methyl]-benzylamine in the prior art, the present invention provides a kind of rec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/04C07C317/28
CPCC07B2200/07C07C231/12C07C231/18C07C315/04C07C317/28C07C233/47
Inventor 石连胜杨波任传栋林泉生
Owner SHANDONG ZOUPING DAZHAN NEW MATERIALS
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