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
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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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