Synthesis method of sec-butyl mercaptan

A sec-butyl mercaptan, synthetic method technology, applied in the direction of mercaptan preparation, organic chemistry, etc., can solve the problem of unretrieved sec-butane mercaptan, and achieve the effect of environmental friendliness

Inactive Publication Date: 2012-04-18
XIAN MODERN CHEM RES INST
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  • Abstract
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  • Claims
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  • Synthesis method of sec-butyl mercaptan

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Embodiment 1

[0015] Add 30ml of water, 7.6g (0.1mol) of thiourea, and 0.2g (0.62mmol) of tetrabutylammonium bromide to the reaction flask, heat up to 50°C under stirring, add 13.7g (0.1mol) of 2-bromobutane, After adding 2-bromobutane, react at 50° C. for 1 hour; the reaction system is heated to 60° C., start to add 12 g (0.3 mol) 20% (weight) NaOH aqueous solution in the reaction flask, and keep 60°C after adding the NaOH aqueous solution. ℃ stirring reaction for 1.5 hours; stop heating, change to distillation apparatus, use 47% (mass) H 2 SO 4 Aqueous solution, adjust the pH of the reaction solution to 1-2, start distillation, the obtained organic layer is dried with anhydrous calcium chloride, filtered, the obtained filtrate is distilled again, and the fraction at 84°C is collected to obtain 7.01g of sec-butylmercaptan. The gas chromatography purity is 99.1%, and the yield is 77.8%.

[0016] Structure Identification:

[0017] Infrared spectrum (potassium bromide): 2923, 2966cm -1 Th...

Embodiment 2

[0021] Add 30ml of water, 7.6g (0.1mol) of thiourea, 0.00685g (0.0212mmol) of tetrabutylammonium bromide to the reaction flask, heat up to 50°C under stirring, add 13.7g (0.1mol) of 2-bromobutane, After adding 2-bromobutane, react at 50°C for 1 hour; heat the reaction system to 60°C, start to add 12g (0.3mol) 20% (weight) NaOH aqueous solution to the flask, and keep 60°C after adding NaOH aqueous solution Stirring reaction 1.5 hours; Stop heating, change distillation unit into, use 47% (mass) H 2 SO 4 Aqueous solution, adjust the pH of the reaction solution to 1 ~ 2, start distillation, the obtained organic layer is dried with anhydrous calcium chloride, filtered, the obtained filtrate is distilled again, and the fraction at 84 ° C is collected to obtain 6.25 g of a colorless liquid, namely sec-butylmercaptan. The gas chromatography purity is 99.0%, and the yield is 68.7%.

Embodiment 3

[0023] Add 30ml of water, 7.6g (0.1mol) of thiourea, and 0.685g (2.12mmol) of tetrabutylammonium bromide to the reaction flask, heat up to 50°C under stirring, add 13.7g (0.1mol) of 2-bromobutane, After adding 2-bromobutane, react at 50°C for 1 hour; heat the reaction system to 60°C, start to add 12g (0.3mol) 20% (weight) NaOH aqueous solution to the flask, and keep 60°C after adding NaOH aqueous solution Stirring reaction 1.5 hours; Stop heating, change distillation unit into, use 47% (mass) H 2 SO 4 Aqueous solution, adjust the pH of the reaction solution to 1-2, start distillation, the obtained organic layer is dried with anhydrous calcium chloride, filtered, the obtained filtrate is distilled again, and the fraction at about 84 ° C is collected to obtain 6.97 g of a colorless liquid. That is, sec-butylmercaptan. The gas chromatography purity is 99.1%, and the yield is 77.4%.

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Abstract

The invention discloses a synthesis method of sec-butyl mercaptan, comprising the following steps of: adding thiourea, a quaternary ammonium salt phase transfer catalyst and water into a reaction bottle, stirring while heating up to the temperature of 50 DEG C, adding 2-bromobutane, reacting at the temperature of 50 DEG C for 1-8 hours after the addition of 2-bromobutane, stirring while heating up to the temperature of 60 DEG C, adding alkali, reacting for 1-8 hours, adjusting pH of the reaction solution to 1-2 by using 47 wt% of an H2SO4 aqueous solution, distilling and collecting fraction of 84 DEG C to obtain sec-butyl mercaptan. The invention is mainly applied for the synthesis of sec-butyl mercaptan.

Description

technical field [0001] The present invention relates to a kind of synthetic method of sec-butyl mercaptan. Background technique [0002] Second-butyl mercaptan is an important chemical raw material and intermediate. At present, the synthesis of mercaptans mainly adopts the sodium hydrosulfide (potassium) method and the thiourea method. The sodium hydrosulfide (potassium) method usually needs to use an autoclave reaction, the operation is complicated, and there are many by-products such as sulfide, so it is not widely used; the thiourea method usually uses bromoalkane and thiourea as raw materials, and passes through The reaction steps of addition, alkali cleavage, and acid neutralization have fewer by-products. For example, the Chinese invention patent CN 1896053A discloses a method for synthesizing mercaptans by thiourea, which includes the steps of addition, cleavage, and neutralization: Add 0.5 moles of 1,2-dibromoethane dropwise to 1 mole of thiourea in hot ethanol (ref...

Claims

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Application Information

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IPC IPC(8): C07C321/04C07C319/02
Inventor 高潮丛志远樊学忠姚依伦杜渭松封利民胡岚
Owner XIAN MODERN CHEM RES INST
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