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Preparation method of 2'-ethylthio ethyl-2-thiol ethyl sulfide

A technology of mercaptoethyl sulfide and dimercaptoethyl sulfide is applied in the field of preparation of sulfide compounds and can solve the problems of low reaction temperature, low yield, low yield and high reaction temperature

Inactive Publication Date: 2016-01-20
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the shortcomings of high reaction temperature and low yield in the synthesis method of 2'-ethylthioethyl-2-mercaptoethyl sulfide in the prior art, the present invention provides a 2'- The preparation method of ethylthioethyl-2-mercaptoethyl sulfide

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  • Preparation method of 2'-ethylthio ethyl-2-thiol ethyl sulfide

Examples

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Embodiment 1

[0018] A. Add 3.08g of dimercaptoethyl sulfide, 200ml of acetonitrile, and then add 3.20g of potassium carbonate and 3.32g of potassium iodide in the reaction flask with Ar gas protection, magnetic stirring, thermometer and reflux device, and react at a temperature of 40°C 1h.

[0019] B. Under Ar gas, slowly drop 200ml of acetonitrile solution containing 2.18g bromoethane into the above-mentioned reaction flask for 6-8 hours; filter after reacting for 3d at a temperature of 40°C, and use 50ml of the mixture obtained by evaporating the filtrate to dryness under reduced pressure. Extract with dichloromethane, wash the extract twice with 10% dilute sulfuric acid, and then wash with distilled water until neutral. The extract was dried over magnesium sulfate and evaporated to dryness under reduced pressure to obtain a colorless liquid crude product, which was separated and purified by a column to obtain 0.81 g of 2'-ethylthioethyl-2-mercaptoethyl sulfide compound with a yield of 2...

Embodiment 2

[0030] A. Add 3.08g of dimercaptoethyl sulfide, 250ml of acetonitrile, and then 3.52g of potassium carbonate and 1.70g of potassium iodide in the reaction flask with Ar gas protection, magnetic stirring, thermometer and reflux device, and react at a temperature of 60°C 2h.

[0031] B. Under Ar gas, slowly drop 150ml of acetonitrile solution containing 2.45g bromoethane into the above-mentioned reaction flask for 6-8h; after reacting for 2d at a temperature of 60°C, filter, and evaporate the filtrate to dryness under reduced pressure in 50ml Extract with dichloromethane, wash the extract twice with 10% dilute sulfuric acid, and then wash with distilled water until neutral. After the extract was dried over magnesium sulfate, it was evaporated to dryness under reduced pressure to obtain a colorless liquid crude product, which was separated and purified by a column to obtain 0.58 g of 2'-ethylthioethyl-2-mercaptoethyl sulfide compound, with a yield of 15.9%.

Embodiment 3

[0033] A. Add 3.08g of dimercaptoethyl sulfide, 160ml of acetonitrile, 4.00g of potassium carbonate and 2.00g of potassium iodide in sequence in a reaction flask equipped with Ar gas protection, magnetic stirring, thermometer and reflux device, and react at a temperature of 50°C for 1.5h .

[0034] B. Under Ar gas, slowly drop 120ml of acetonitrile solution containing 2.60g bromoethane into the above-mentioned reaction flask for 6-8 hours; after reacting for 1d at a temperature of 50°C, filter, and evaporate the filtrate to dryness under reduced pressure in 50ml Extract with dichloromethane, wash the extract twice with 10% dilute sulfuric acid, and then wash with distilled water until neutral. After the extract was dried over magnesium sulfate, it was evaporated to dryness under reduced pressure to obtain a colorless liquid crude product, which was separated and purified by a column to obtain 0.62 g of 2'-ethylthioethyl-2-mercaptoethyl sulfide compound, with a yield of 17.0%. ...

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Abstract

The invention discloses a preparation method of 2'-ethylthio ethyl-2-thiol ethyl sulfide. The method comprises the following steps that dimercaprol ethyl sulfide is used as a raw material; under the protection of inert atmosphere, potassium carbonate is used as an acid-binding agent to take reaction with bromoethane to obtain 2'-ethylthio ethyl-2-thiol ethyl sulfide; the 2'-ethylthio ethyl-2-thiol ethyl sulfide is mainly used as a midbody of long-chain aza-thioether. The method has the advantages that the reaction temperature is low; the yield is higher; the selectivity is good.

Description

technical field [0001] The present invention relates to a kind of preparation method of thioether compound, relate in particular to a kind of preparation method of 2'-ethylthioethyl-2-mercaptoethyl sulfide. Background technique [0002] Thioether compounds, especially azathioethers, not only have metal chelation and coordination, but also can combine with other functional molecules or materials through nitrogen atoms, and have application prospects in sensors and selective enrichment of heavy metals. The patent "Mercuryiondetectionsensorusingphosphorescence, mercuryiondetectionsensorarraycontainingit, anditsmanufacturemethod, KR2010106005" discloses that it has -SC 2 h 4 -NH-C 2 h 4 Molecules of S-structure (ie, SNS) units are used in mercury ion sensors. Its precursor is S-C of single-ended thiol 2 h 4 - the thioether compound, the document ("Synthesisandmetal-ionbindingpropertiesofmonoazathiacrownethers"JournalofOrganicChemistry[J].2001,66(21):7008-7012) also disclos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C321/14C07C319/14
Inventor 纪晓唐葛忠学李陶琦丁可伟仝敏超苏海鹏肖啸刘庆刘愆
Owner XIAN MODERN CHEM RES INST