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The preparation method of 3-mercapto-1-propanol

A technology of mercaptopropionic acid and propanol, which is applied in the field of preparation of 3-mercapto-1-propanol, can solve the problems of high price of tetrahydroaluminum lithium, limited industrial application, harsh reaction conditions, etc., and achieves low pollution and low price. , mild conditions

Active Publication Date: 2019-03-15
三门峡奥科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] This process is relatively thorough in reduction, but the price of lithium tetrahydrogen used is relatively high, it is flammable and explosive, and the reaction conditions are harsh, so its industrial application is limited.

Method used

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  • The preparation method of 3-mercapto-1-propanol
  • The preparation method of 3-mercapto-1-propanol
  • The preparation method of 3-mercapto-1-propanol

Examples

Experimental program
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Effect test

Embodiment 1

[0022] A preparation method of 3-mercapto-1-propanol, comprising the steps of: adding 50ml of tetrahydrofuran and 10.6g of 3-mercaptopropionic acid into a reaction kettle successively, adding 5.7g of sodium borohydride in batches at 10-20°C, and continuously Stir, continue to stir for 30 minutes after the sodium borohydride is added dropwise, then slowly add 11.5g of boron trifluoride tetrahydrofuran solution dropwise at this temperature; raise the temperature to 35°C and keep it for 5 hours, then raise the temperature to 50°C and keep it for 1 hour, When the reaction mixture becomes solid, cool down to room temperature, slowly add 30ml of water, then distill off tetrahydrofuran, add 9.1g of hydrochloric acid (33%wt) to the remaining mixture, adjust the pH to 2~3; add 20ml of chloroform to stir, suction filter, filter cake The boric acid crystals were obtained by recrystallization, and the filtrate was separated with a separatory funnel; the water phase was extracted twice with...

Embodiment 2

[0024] A preparation method of 3-mercapto-1-propanol, comprising the steps of: adding 50ml of tetrahydrofuran and 10.6g of 3-mercaptopropionic acid into a reaction kettle successively, adding 6.4g of sodium borohydride in batches at 10-20°C, and continuously Stir, continue stirring for 30 minutes after the sodium borohydride is added dropwise, then slowly add 12.8g of boron trifluoride tetrahydrofuran solution dropwise at this temperature; raise the temperature to 30°C and keep it for 4 hours, then raise the temperature to 55°C and keep it for 1.2 hours, When the reaction mixture is solid, lower it to room temperature, slowly add 30ml of water dropwise, distill off tetrahydrofuran after dropping, add 10.0g of hydrochloric acid (33%wt) to the remaining mixture, adjust the pH to 2~3; add 20ml of chloroform to stir, and filter with suction , the filter cake was recrystallized to obtain boric acid crystals, and the filtrate was separated with a separatory funnel; the water phase wa...

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Abstract

The invention relates to a preparation method of 3-mercapto-1-propanol. The preparation method is characterized in that 3-mercapto-1-propanol is prepared from 3-mercaptopropionic acid as a raw material, tetrahydrofuran as a solvent and a NaBH4 / BF3 system as a reducing agent by controlling reaction conditions, a solution obtained after the reaction is heated, a solid mixture is obtained and subjected to post-processing, and a finished product of 3-mercapto-1-propanol is obtained, wherein the optimal mole ratio of 3-mercaptopropionic acid, NaBH4 and a boron trifluoride tetrahydrofuran complex is 1:(1.5-1.7):(0.8-1.0). Compared with other preparation methods of 3-mercapto-1-propanol, the preparation method of 3-mercapto-1-propanol has the beneficial effects that the raw materials are lower in cost, and the cost is reduced; the reaction conditions are mild, the reaction is simple and feasible, and the operation process is safe; the yield of 3-mercapto-1-propanol can reach 80% or higher, and the product purity can reach 99.3% or higher; little pollution is caused in the preparation process, all used organic solvents can be recycled, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 3-mercapto-1-propanol. Background technique [0002] 3-Mercapto-1-propanol is an important intermediate in the preparation of medicine, pesticide and electronic materials. In industry, 3-mercapto-1-propanol is an important fine chemical raw material. Therefore, 3-mercapto-1-propanol has a good market prospect. [0003] At present, the preparation method of 3-mercapto-1-propanol mainly contains three kinds: [0004] One is to use 3-chloro-1-propanol as raw material (Journal of American Chemical Society, 67,594-597,1945), react with thiourea to prepare isothiourea intermediate, and then hydrolyze in alkaline aqueous solution to obtain 3-mercapto -1-propanol. Its reaction formula is as follows: [0005] [0006] The disadvantage of this process is that the raw materials are expensive, the cost is high, the yield is low (about 40%), ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/12C07C319/12
CPCC07C319/12C07C323/12
Inventor 赵松芳兀吉康兀江刘之华尚晓东郭超霞袁淑芳
Owner 三门峡奥科化工有限公司