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Method for preparing formamidine acetate

A technology for formamidine acetate and acetate, applied in the field of preparing formamidine acetate, can solve the problems of being unsuitable for industrialized large-scale production and high cost, and achieve the effects of low cost, little environmental pollution and high yield

Inactive Publication Date: 2010-06-02
YINGKOU YINGXIN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is reported more, OGURA NAOHITO etc. in Jpn.Kokai Tokkyo Koho, 2005126332; ITTERVON FRANZ-ALBERT etc. in Ger.Offen., 4001160; and THEIS CHRISTOPH et al. reported in Ger.Offen., 4422273, orthoformic acid three Methyl ester is mixed with acetic acid, and in the presence of different temperatures and solvents, ammonia gas is introduced, the yield is 84-95%, the product has high purity, and the preparation method is simple. The cost is very high, this method is only suitable for laboratory preparation, not suitable for industrial production

Method used

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  • Method for preparing formamidine acetate
  • Method for preparing formamidine acetate
  • Method for preparing formamidine acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 500ml reaction bottle, add 200ml of solvent and 46g of ethanol, stir and cool down to below -15°C, add 27g of hydrocyanic acid, start to pass in 40g of dry hydrogen chloride gas, control the temperature not to exceed -5°C for 6 hours, filter to obtain Urethane hydrochloride.

[0024] Dissolve 85g of ammonium acetate in 200ml of absolute ethanol, add the ethyl imidoformate hydrochloride obtained in the previous step in portions below -5°C, stir vigorously for 1 hour, raise the temperature to room temperature for 1 hour, then raise the temperature to 45°C to continue After reacting for 1 hour, white precipitated ammonium chloride gradually precipitated, cooled down, and filtered.

[0025] The filtrate is heated to reflux, and at the same time, dry ammonia gas is introduced at a certain speed for 1.5 to 2 hours, and about 35g of ammonia gas is introduced, and white solids are gradually precipitated in the reaction bottle. After cooling down, filtering, and washing wit...

Embodiment 2

[0027] In a 500ml reaction bottle, add 200ml of solvent and 37g of methanol, stir and cool down to below -20°C, add 27g of hydrocyanic acid, start to pass in 42g of dry hydrogen chloride gas, control the temperature not to exceed -0°C for 8 hours, filter to obtain Methyl carbamate hydrochloride.

[0028] Dissolve 93g of ammonium acetate in 200ml of anhydrous methanol, add the methyl imidoformate hydrochloride obtained in the previous step in portions below -5°C, stir vigorously for 1 hour, raise the temperature to room temperature and react for 2 hours, then raise the temperature to 40°C to continue After reacting for 1 hour, white precipitated ammonium chloride gradually precipitated, cooled down, and filtered.

[0029] The filtrate is heated to reflux, and at the same time, dry ammonia gas is introduced at a certain speed for 2 to 2.5 hours, and about 85g of ammonia gas is introduced, and a white solid is gradually precipitated in the reaction bottle. After cooling down, fil...

Embodiment 3

[0031] Into a 500ml reaction bottle, add 200ml of solvent and 46g of ethanol, stir and cool down to below -5°C, add 27g of hydrocyanic acid, start to pass in 40g of dry hydrogen chloride gas, control the temperature not to exceed 0°C for 6 hours, filter to obtain imine Ethyl formate hydrochloride.

[0032] Dissolve 78g of ammonium acetate in 200ml of absolute ethanol, add the ethyl imidoformate hydrochloride obtained in the previous step in portions below -5°C, stir vigorously for 1 hour, raise the temperature to room temperature for 1 hour, and then raise the temperature to 45°C to continue After reacting for 1 hour, white precipitated ammonium chloride gradually precipitated, cooled down, and filtered.

[0033] The filtrate is heated to reflux, and at the same time, dry ammonia gas is introduced at a certain speed for 1.5 to 2 hours, and about 45g of ammonia gas is introduced, and white solids are gradually precipitated in the reaction bottle. After cooling down, filtering, ...

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Abstract

The invention relates to a method for preparing formamidine acetate. The method comprises the following steps of: according to a molar ratio of 1.0:(0.9-1.5):(0.9-1.5):(1.0-2.0):(2.0-5.0) of formonitrile to anhydrous fatty alcohol to anhydrous hydrogen chloride to ammonium acetate to ammonia, generating a hydrochloride of alkyl carbamate by the formonitrile, the anhydrous fatty alcohol and the anhydrous hydrogen chloride; generating ammonium chloride and an acetate of the alkyl carbamate by exchanging with the ammonium acetate without generating orthoformic acid trialkyl ester through alcoholysis; and continuously ammoniating the acetate of the alkyl carbamate to generate the formamidine acetate. In the reaction process of the method, the raw materials do not contain the orthoformic acid trialkyl ester, thus the reaction process has simple operation, low cost, less environmental pollution and high yield.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for preparing formamidine acetate. Background technique [0002] Formamidine acetate, white crystal, melting point 162~164℃. It is mainly used for the synthesis of the intermediate 4-hydroxy-5-fluoropyrimidine of the drug Fuxeridine, and it can also be used for the synthesis of biologically active antineoplastic drugs and antifungal drugs containing pyrimidine rings. It has broad development prospects and application value. According to bibliographical reports, the synthesis of formamidine acetate mainly contains the following methods: [0003] 1. Catalytic hydrogenation of amines. WEISS STEFAN DR et al. reported in Ger.Offen., 3808767, in the presence of acetic acid, use catalyst catalytic hydrogenation, reduce cyanamide to obtain formamidine acetate, in this environment the catalyst is easily dissolved in the solution, resulting in dark product color, can not be obta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/12C07C53/08
Inventor 高庆昌
Owner YINGKOU YINGXIN CHEM TECH CO LTD
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