Preparation method for creatinol sulphate

The technology of inositol sulfate and concentrated sulfuric acid is applied in the field of preparation of inositol sulfate, can solve the problems of polluted environment, large consumption of organic solvent and high production cost, achieves good purity, simple and easy post-processing, and low cost Effect

Inactive Publication Date: 2010-03-17
TIANJIN TIANCHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the technical problems of producing toxic gas, polluting the environment, excessive consumption of organic solvents and high

Method used

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  • Preparation method for creatinol sulphate
  • Preparation method for creatinol sulphate

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 77 mL (0.55 mol) of an aqueous solution containing 23 g of cyanamide and 20 mL (0.5 mol) of methanol into a 250 mL four-neck flask, add 26 g (0.26 mol) of 98% concentrated sulfuric acid dropwise, and stir at room temperature for 60 min after adding sulfuric acid. Then, 37.5 g (0.5 mol) of N-methylaminoethanol was added, and after the addition was completed, the temperature was raised at 60° C. for 5 h. After the reaction was completed, it was concentrated under reduced pressure. Add 100mL of absolute ethanol while stirring at 50°C, the formed myo-sulphate precipitates out as granular crystals, filter the precipitated crystals after cooling, wash with absolute ethanol, and dry. The yield is 60-70%. Product purity reaches 93-99%

Embodiment 2

[0022] Add 70 mL (0.5 mol) of aqueous solution containing 21 g of cyanamide and 20 mL (0.5 mol) of methanol into a 250 mL four-neck flask, add 25 g (0.25 mol) of 98% concentrated sulfuric acid dropwise, and stir at room temperature for 60 min after adding sulfuric acid. Then, 37.5 g (0.5 mol) of N-methylaminoethanol was added, and after the addition was completed, the temperature was raised at 70° C. for 4 h. After the reaction was completed, it was concentrated under reduced pressure. When the temperature is lowered to 60°C, add 200ml of acetone under stirring, and the generated myo-sulphate precipitates in the form of granular crystals. After cooling, filter the precipitated crystals, wash them with absolute ethanol, and dry them. The yield is 65-70%. The product purity reaches 93-99%.

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Abstract

The invention relates to a preparation method for 1-methyl-1-(beta-hydroxy ethyl) guanidine sulfate (creatinol sulphate), belonging to the preparation method for guanidine derivatives. The preparation method for creatinol sulphate comprises the following steps: (1) cyanamide aqueous solution, methyl alcohole and concentrated sulfuric acid reacting in the temperature of 10 DEG C to 40 DEG C for 30min to 90 min; (2) dropwise adding N-methyl amino-alcohol into the solution in the step (1), reacting for 3h-5h in the temperature of 30-80 DEG C, decompressing and concentrating; (3) adding organic solvent into the concentrated solution, separating out creatinol sulphate and crystallizing, and obtaining creatinol sulphate finished product after washing and drying. The preparation method has mildreactive conditions, is simple and convenient to operate and practical, has low toxicity owing to taking water as solvent, low cost and low vitality, simultaneously is simple and practical in the post treatment, and saves time and energy. The obtained product has high yield and good purity; and the purity of the product can reach 93%-99%.

Description

Technical field: [0001] The invention relates to a preparation method of guanidine derivatives, in particular to a preparation method of inositol sulfate with low toxicity and low cost. Background technique: [0002] The chemical name of inositol sulfate is 1-methyl-1-(β-hydroxyethyl)guanidine sulfate, and the molecular formula is C 8 h 24 N 6 o 6 S, molecular weight 332.37, CAS registration number 50648-53-8, English name: creatinol sulfate; N-(2-Hydroxyethyl)-N-methylguanidine sulfate. The structural formula is as follows: [0003] [0004] Myo-inositol is an important intermediate in organic synthesis. Myo-inositol can exist in various forms, such as myo-sulphate, hydroiodide and hydrobromide, and its various derivatives can be used as energy supplements agents, food additives and plant growth regulators. [0005] The preparation method of the disclosed myo-sulphate of French patent FR.2162262 is to react with S-methylisothiourea-sulphate and N-methylaminoethanol...

Claims

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Application Information

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IPC IPC(8): C07C279/08C07C277/08
Inventor 张国基
Owner TIANJIN TIANCHENG PHARMA
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