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Method for producing bromo butyric acid

A technology of bromobutyric acid and hydrogen bromide, which is applied in the preparation of carboxylate/lactone, organic chemistry and other directions, can solve the problems of high material concentration, cannot meet the requirements of the pharmaceutical industry, and is not easy to consume, and achieves a simple and easy process. Forming the effect of large-scale production and wide application prospects

Inactive Publication Date: 2006-04-19
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that no organic solvent is used, the concentration of the material in the system is too high, and it is difficult to stir, and the last remaining part of the raw material γ-butyrolactone is not easy to consume and remains in the system
It is difficult to obtain high-purity 4-bromobutyric acid, which cannot meet the requirements of the pharmaceutical industry
Therefore, this method also has disadvantages in technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: in the three-necked bottle of 500 milliliters, install thermometer, stirrer, add raw material γ-butyrolactone (1 mole, 86 grams), normal hexane (200 milliliters), start to stir then. Dry hydrogen bromide gas (1.1 mol, 89 g) was introduced, and the reaction temperature was controlled at 10°C~20°C. After completion of the hydrogen bromide gas sparging, the mixture was stirred at this temperature for an additional 2 hours. Then cool to 0~10°C, stir, and a large number of crystals are formed. After filtration, a light yellow solid of 4-bromobutyric acid was obtained, weighing 160 g, with a yield of 96% and a purity of 99.2% (gas chromatography analysis).

Embodiment 2

[0015] Embodiment 2: in the three-necked bottle of 500 milliliters, install thermometer, stirrer, add raw material γ-butyrolactone (1 mole, 86 grams), then start to stir. Dry hydrogen bromide gas (1.2 mol, 97 g) was introduced, and the reaction temperature was controlled at 30°C~40°C. After completion of the hydrogen bromide gas sparging, it was stirred at this temperature for an additional 4 hours. Then cool to 0~20°C, stir, and a large number of crystals are formed. After filtration, a light yellow 4-bromobutyric acid solid was obtained, with a weight of 164 g, a yield of 98%, and a purity of 99.5% (gas chromatography analysis).

Embodiment 3

[0016] Embodiment 3: in the three-necked bottle of 500 milliliters, install thermometer, stirrer, add raw material γ-butyrolactone (1 mole, 86 grams), toluene (200 milliliters), begin to stir then. Dry hydrogen bromide gas (1.3 mol, 105 g) was introduced, and the reaction temperature was controlled at 40°C~50°C. After completion of the hydrogen bromide gas sparging, the mixture was stirred at this temperature for an additional 5 hours. Then cool to 0~20°C and stir for 2 hours, a large amount of crystals are formed. After filtration, a light yellow 4-bromobutyric acid solid was obtained, weighing 162 g, with a yield of 97% and a purity of 99.0% (gas chromatography analysis).

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PUM

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Abstract

A process for preparing 4-bromobutanoic acid includes such steps as filling the dried hydrogen bromide gas in the organic solvent containing gamma-butyrolactone, ring opening reaction to generate 4-bromobutanoic acid, cooling to the temp lower than 30 deg.C, crystallizing, depositing and filtering. Its advantage is high purity.

Description

technical field [0001] The invention belongs to the technical field of organic compounds, and in particular relates to a preparation method of 4-bromobutyric acid. Background technique [0002] 4-Bromobutyric acid is a very important pharmaceutical intermediate. At present, there is no domestic manufacturer producing it. The reason is that it is difficult to obtain high-purity products due to insufficient technology. Since the melting point of 4-bromobutyric acid is low, that is, the melting point is 32-33 ° C, and it is not easy to form crystals. Generally, 4-bromobutyric acid is obtained by distillation. In the presence of water, 4-bromobutyric acid is easily dehydrobrominated by cyclization to generate γ-butyrolactone. Therefore, in the distillation process, a part of 4-bromobutyric acid reacts with water in the system and becomes γ-butyrolactone, which is difficult to obtain high-purity 4-bromobutyric acid. [0003] R.G.Ainsi (Bull.Société Chim.de France, 1975, Page 8...

Claims

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Application Information

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IPC IPC(8): C07C51/09C07C53/19
Inventor 刘国斌
Owner FUDAN UNIV
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