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Synthesis method of 2, 2-ethoxyethanol

A technology of diethoxyethanol and diethoxyethyl acetate is applied in the synthesis field of antiviral drug lamivudine raw material 2, and can solve the problems of side reaction, low product purity and yield, etc., Achieving the effect of full reaction, high product yield and lower production cost

Inactive Publication Date: 2011-07-06
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method technological process is simple; The method is prone to other side reactions, and the purity and yield of the final product are lower

Method used

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  • Synthesis method of 2, 2-ethoxyethanol
  • Synthesis method of 2, 2-ethoxyethanol
  • Synthesis method of 2, 2-ethoxyethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Put 400g of methyl dichloroacetate, 400ml of water and 40g of hydrochloric acid with a concentration of 36.5% into a 1000ml four-neck flask, raise the temperature to 80°C, and perform a hydrolysis reaction for 2 hours. After about 80g of water and methanol, use vacuum distillation to control the temperature below 100°C, and distill the water in the reaction system. , Collect the distilled fractions to obtain dichloroacetic acid.

[0036] Put 75g of dichloroacetic acid, 861g of 17.4% sodium ethoxide and 230g of absolute ethanol into a 1000ml four-neck flask, heat up to 80°C for reflux, and react for 4.5 hours. After the reaction, cool down to 0°C and start to drop 37 % Hydrochloric acid ethanol solution 127.5g, add dropwise, control the temperature below 10°C, after the dropwise addition is completed, heat up to 20°C for reaction, after the reaction, then cool down to 0°C, adjust the pH value to 6.8 with sodium ethylate, the whole During the pH adjustment process, contr...

Embodiment 2

[0039] Put 400g of methyl dichloroacetate, 400ml of water and 120g of 30.0% hydrochloric acid into a 1000ml four-neck flask, heat up to 80°C, and perform hydrolysis reaction for 4 hours. After about 100g of water and methanol, switch to vacuum distillation to control the temperature below 100°C, and distill the water in the reaction system. The distilled fractions are dichloroacetic acid.

[0040] Put 75g of the prepared dichloroacetic acid, 600g of 15% sodium ethoxide and 250g of absolute ethanol into a 1000ml four-necked bottle, raise the temperature to 76°C-80°C, and react for 6 hours. After the reaction, cool down to 0°C and start dripping Add 90g of hydrochloric acid ethanol solution with a concentration of 40%, and control the temperature below 10°C. After the dropwise addition, raise the temperature to 20°C for reaction. During the process, the temperature was controlled not to exceed 10°C. After adjustment, the stirring was continued for 1 hour, and the sodium chlorid...

Embodiment 3

[0043] Put 400g of ethyl dichloroacetate, 400ml of water and 50g of hydrochloric acid with a concentration of 35.0% into a 1000ml four-necked flask, heat up to 80°C, and perform a hydrolysis reaction for 3 hours. After the reaction, distill under normal pressure to remove the residual dichloroacetic acid After about 110g of ethyl ester, water and ethanol, switch to vacuum distillation, control the temperature to less than 100°C, and distill out the water in the reaction system. When the temperature is above ℃, collect the distilled fractions to obtain dichloroacetic acid.

[0044] Put 75g of the prepared dichloroacetic acid, 870g of 18% sodium ethoxide and 230g of absolute ethanol into a 1000ml four-necked bottle, raise the temperature to 70°C to 75°C, and react for 6 hours. After the reaction, cool down to 0°C and start dripping Add 140g of hydrochloric acid ethanol solution with a concentration of 30%, and control the temperature below 10°C. After the dropwise addition, rais...

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Abstract

The invention relates to a synthesis method of 2, 2-ethoxyethanol, belonging to the technical field of medicine and chemical industry. The method comprises the steps of: taking compound of a formula (I) as a raw material, and hydrolytically reacting the raw material with inorganic acid to obtain dichloroacetic acid; reacting the obtained dichloroacetic acid with caustic alcohol in absolute ethyl alcohol in a backflow way, adding hydrochloric acid ethanol solution in a cooling way after the reaction, adjusting PH value, filtering and distilling to obtain 2, 2-ethyl diethoxyacetate; and reacting the 2, 2-ethyl diethoxyacetate obtained in step b with KBH4 and inorganic catalyst in inorganic catalyst in a backflow way to obtain the 2, 2-ethoxyethanol. The synthesis method has the advantages that the raw material is easily obtained, the technical process is simple, the reaction condition is stable, the reaction can be performed without high pressure, and the synthesis method is suitable for the industrial production on a large scale. The solvent ethanol can be recovered and used mechanically, the atom economy is good, the cost is low, the product yield is high, and the product quality is more than 98%.

Description

technical field [0001] The invention relates to a method for synthesizing a drug raw material, in particular to a method for synthesizing an antiviral drug lamivudine raw material 2,2-diethoxyethanol, which belongs to the technical field of medicine and chemical industry. Background technique [0002] 2,2-diethoxyethanol is an important raw material for the synthesis of the intermediate 1,3-oxathione-5-one compound of the antiviral drug lamivudine, and has an important role in the fields of organic synthesis and drug synthesis. Value. [0003] The molecular formula of 2,2-diethoxyethanol is C 6 h 14 o 3 , the molecular weight is 134.17. Its structural formula is [0004] [0005] In the prior art, the synthesis of 2,2-diethoxyethanol mainly includes the following schemes. Scheme 1: As William E.Parham et al. disclosed in J.Am.Chem.Soc., 1955,77 (23), 6391-6393, react with sodium to synthesize sodium phenethylate with phenylethyl alcohol raw material, and then react ...

Claims

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Application Information

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IPC IPC(8): C07C43/315C07C41/48
Inventor 孙佰申汪一波金召磊潘富友
Owner TAIZHOU UNIV
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