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Method utilizing methyl sodium sulfate offscum to synthesize S-methyl-iso-thiourea sulfate

A technology of methylisothiouronium sulfate and sodium methylsulfate, which is applied in the direction of organic chemistry, can solve the problems of high price, generation of malodorous gas, low product yield, etc., meet low requirements for reaction conditions, solve pollution problems, The effect of high product yield

Active Publication Date: 2013-12-25
ZHEJIANG DAYANG BIOTECH GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of methyl halide as a methylation reagent has major disadvantages, such as methyl iodide is expensive, and methyl chloride is a gas, which increases the difficulty of controlling the reaction and makes it difficult for industrial production
[0009] (2) cothermal reaction of hydrochloric acid aqueous solution of thiourea and alcohol: when thiourea was prepared in the cothermal reaction of hydrochloric acid aqueous solution of alcohol to S-methylisothiourea, more by-products were generated in the reaction, resulting in low product yield and poor quality Inferior disadvantages, so industrial production cannot be realized
This method has the advantages of simple process, feasible technology and stable operation, but it will produce malodorous gas and high-concentration salt-containing organic wastewater during the production process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1, a kind of method utilizing sodium methylsulfate waste residue to synthesize S-methylisothiourea sulfate, carries out following steps successively:

[0052] 1) Add 152ml of water and 152g (2mol) of thiourea into a 1000ml three-necked reaction flask, raise the temperature to 80°C and stir until the thiourea is completely dissolved to obtain a thiourea solution.

[0053] 2) Slowly add 319g of solid sodium methyl sulfate waste residue (sodium methyl sulfate 2.2mol) to the thiourea solution obtained in step 1) (the addition is completed in about 10-20 minutes), and raise the temperature to 105-115°C to make Its reflux reaction 2h.

[0054] 3) Cool the reacted material obtained in step 2) to 40°C (at this time, the reacted material does not solidify), control the stirring speed at 50-100 rpm, and slowly add 304ml of methanol for crystallization.

[0055] 4), the material obtained after crystallization in step 3) is separated from solid and liquid by a centrifug...

Embodiment 2

[0063] Embodiment 2, a kind of method utilizing sodium methylsulfate waste residue to synthesize S-methylisothiourea sulfate, carries out following steps successively:

[0064] 1) Add 304ml of water and 152g (2mol) of thiourea into a 1000ml three-necked reaction flask, raise the temperature to 80°C and stir until the thiourea is completely dissolved to obtain a thiourea solution.

[0065] 2) Slowly add 436 g of solid sodium methyl sulfate waste residue (3 mol of sodium methyl sulfate) to the thiourea solution obtained in step 1), raise the temperature to 105-115 ° C, and allow it to reflux for 2 hours.

[0066] 3) Cool the reaction material liquid obtained in step 2) to 40°C (the reaction material liquid does not solidify at this time), control the stirring speed at 50-100 rpm, and slowly add 608ml of methanol for crystallization.

[0067] 4), the material obtained after the crystallization in step 3) was subjected to solid-liquid separation through a centrifuge, and 405 g of ...

Embodiment 3

[0076] Embodiment 3, a kind of method utilizing sodium methylsulfate waste residue to synthesize S-methylisothiourea sulfate, carries out following steps successively:

[0077] 1) Add 152ml of water and 152g (2mol) of thiourea into a 1000ml three-necked reaction flask, raise the temperature to 80°C and stir until the thiourea is completely dissolved to obtain a thiourea solution.

[0078] 2) Add 290 g of solid sodium methyl sulfate waste residue (2 mol of sodium methyl sulfate) to the thiourea solution obtained in step 1), raise the temperature to 105-115 ° C, and allow it to reflux for 2 hours.

[0079] 3) Cool the reaction material liquid obtained in step 2) to 40°C (at this time, the reaction material does not solidify), control the stirring speed at 50-100 rpm, and slowly add 304ml of methanol for crystallization.

[0080] 4), the material obtained after the crystallization in step 3) was separated from solid and liquid by a centrifuge, and 380 g of solid material (a mixtu...

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Abstract

The invention discloses a method utilizing methyl sodium sulfate offscum to synthesize S-methyl-iso-thiourea sulfate. Methyl sodium sulfate offscum and thiourea are taken as fundamental raw materials, water is taken as the solvent, and reflux reaction is performed under the neutrality condition to obtain the S-methyl-iso-thiourea sulfate, of which the reaction formula is 2(H2N)2C=S + 2CH3OSO3Na react to generate (HN=C(SCH3)NH2)2,H2SO4+Na2SO4. The methyl sodium sulfate offscum, a by-product with the content of larger than or equal to 90%, obtained through producing hemiacetal or vitamin B1, and thiourea are taken as initial raw materials, water is taken as the solvent, and reaction is performed under the neutrality condition to prepare the end product. The method has the characteristics of high reaction speed, low demand on reaction conditions, good product quality, high product yield and the like; water replaces an organic solvent, and the methyl sodium sulfate offscum replaces a highly toxic product (methyl sulfate) to serve as a methylate raw material, so that not only is the advantage of low cost is achieved, but also the difficult pollution problem of the methyl sodium sulfate offscum is solved; only methanol is taken as a crystallization solvent and is recyclable for repeated use in the production process; waste water and other offscums are not produced in the production process, so that comprehensive utilization of the methyl sodium sulfate offscum and green production are realized.

Description

technical field [0001] The invention belongs to the fields of fine chemical industry and environmental protection, and relates to the synthesis technology of fine medicine intermediates, in particular to a technology for synthesizing S-methylisothiouronium sulfate by using sodium methyl sulfate waste residue. Background technique [0002] S-methylisothiouronium sulfate is an important intermediate in organic synthesis, used in the pharmaceutical industry to produce anticancer drugs (such as 5-fluorouracil, propiguanidine and hydroxyguanidine sulfate), antihypertensive drug guanidinol, etc. ; In the pesticide industry, it is used in the production of fungicides carbendazim, benomyl and the insecticide pirimiphos-methyl, etc.; it is also an intermediate for the preparation of guanethidine sulfate and prednisolone sodium phosphate. [0003] The U.S. invention patent Preparation for producing creatine or creatine monohy drate (USA, 6326513) applied by Li hua et al. discloses a m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/32
Inventor 王国平徐旭辉陈阳贵汪贤玉涂永福关卫军
Owner ZHEJIANG DAYANG BIOTECH GROUP