Preparation method of sodium n-propyl thiosulfate

A technology of propyl sodium thiosulfate and sodium thiosulfate, which is applied in the field of medicine and chemical industry, can solve the problems of long preparation time, long reaction time, and high consumption of polyethylene glycol, so as to reduce reaction time, reduce consumption, and save cost effect

Inactive Publication Date: 2012-01-04
江苏兄弟维生素有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the amount of polyethylene glycol 400 required for the preparation of the above-mentioned intermediate

Method used

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  • Preparation method of sodium n-propyl thiosulfate

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Effect test

Embodiment 1

[0019] 1. Add 74.5g of sodium thiosulfate pentahydrate to the high-speed shear reactor, dissolve it with an equal amount of distilled water, then add polyethylene glycol 400, 1.5g, n-bromopropane 44g, and adjust the speed to 7000r / min~8000r / min , heated to reflux, and reacted for 2 hours.

[0020] 2. After the reaction was completed, the content of n-propyl sodium thiosulfate was analyzed to be 27%, and the yield was 98% (calculated as sodium thiosulfate).

Embodiment 2

[0022] 1. Add 74.5g of sodium thiosulfate pentahydrate into the high-speed shear reactor, dissolve it with an equal amount of distilled water, then add 400, 2g of polyethylene glycol, 44g of n-bromopropane, and adjust the speed to 6000r / min~7000r / min. Heat to reflux and react for 2 hours.

[0023] 2. After the reaction was completed, the content of n-propyl sodium thiosulfate was analyzed to be 26%, and the yield was 95% (calculated as sodium thiosulfate).

Embodiment 3

[0025] 1. Add 74.5g of sodium thiosulfate pentahydrate into the high-speed shear reactor, dissolve it with an equal amount of distilled water, then add polyethylene glycol 400, 1g, n-bromopropane 44g, adjust the speed to 8000r / min~10000r / min, Heat to reflux and react for 2 hours.

[0026] 2. After the reaction was completed, the content of n-propyl sodium thiosulfate was analyzed to be 26.5%, and the yield was 96.5% (calculated as sodium thiosulfate).

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Abstract

The invention discloses a preparation method of sodium n-propyl thiosulfate. The preparation method of sodium n-propyl thiosulfate comprises the following steps: adding sodium thiosulfate pentahydrate in a high-speed shearing reactor, and dissolving sodium thiosulfate pentahydrate with equivalent distilled water, wherein the rotation speed of the high-speed shearing reactor is 6000-10000 r/min; and then adding polyethylene glycol 400 and n-propyl bromide, and reacting through heating and refluxing. The preparation method has the beneficial effects that a sodium thiosulfate aqueous solution reacts with n-propyl bromide, wherein the former is the aqueous solution, and the latter is an organic phase, so the sodium thiosulfate aqueous solution is immiscible with the organic phase; and polyethylene glycol 400 is a phase transfer catalyst so that the two phases which are immiscible originally are miscible in a certain degree, thereby effectively promoting the reaction to conduct, reducing the amount of polyethylene glycol 400, saving cost and shortening reaction time.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a preparation method of n-propyl sodium thiosulfate. Background technique [0002] There are two synthetic methods of prothiamine, the first method is to prepare by mixing thiamine and garlic juice; the post-processing of this method is cumbersome and the yield is very low. [0003] The second method uses NB1 as a raw material, and the hydrolyzate is hydrolyzed, and then condensed with n-propyl sodium thiosulfate to obtain prothiamin. This method is simple and easy, and the raw material is cheap and easy to obtain. Its synthetic route is as follows: [0004] [0005] The preparation process of the above-mentioned intermediate n-propyl sodium thiosulfate is as follows, sodium thiosulfate pentahydrate and pure water are dissolved under stirring, then polyethylene glycol 400 and 1-bromopropane are added, and steam is heated to reflux for 5 Hours, lower the temperat...

Claims

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Application Information

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IPC IPC(8): C07C381/00
Inventor 李健平李来成陈英明
Owner 江苏兄弟维生素有限公司
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