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A process for splitting pantolactone to prepare optically active pantolactone

A pantolactone and optical activity technology is applied in the field of preparation of pantolactone, which can solve the problems of complex production process, complicated preparation and recovery of splitting reagents, and high production cost, so as to reduce production cost and avoid splitting. Difficulty in reagent recovery, easy to produce effects

Active Publication Date: 2022-05-03
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional industrial methods for preparing D-pantolactone are chemical resolution and biological resolution. These two methods have complex production processes, tedious preparation and recycling of resolution reagents, and high production costs; the patented method of induced resolution ZL201110097950.7 So far no industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Seed preparation

[0038] In a 50-liter pilot test kettle, put 15 kg of water, 10 kg of sodium sulfate, and 15 kg of D-(-)-pantolactone with a standard specific optical rotation higher than 48.5, start stirring, heat up to 85°C to dissolve, and keep warm for half a day. Hour. The temperature was lowered to 15°C, and the material was discharged by centrifugation to obtain 15 kg of crystals and 24 kg of filtrate.

[0039] to split

[0040] Mix 27000g of DL-pantolactone, 2450g of methanol and 324g of water to obtain a pantolactone solution with a water content of 1.09% and a concentration of 90.7% by mass, which is heated to 60°C for dissolution. Under stirring conditions, add 405g of 50-400 mesh D-(-)-pantolactone crystals to the above solution at 15°C as seed crystals, keep stirring at a temperature of 9-13°C, and monitor the optical rotation during stirring , the specific method is: sampling and suction filtration, filling the filtrate into a 10cm optical rotation tu...

Embodiment 2

[0042] Seed preparation

[0043] Put 15 kg of water, 12 kg of ammonium bisulfate, and 15 kg of L-(+)-pantolactone with a standard specific rotation higher than 48.5 into a 50-liter pilot test kettle, start stirring, heat up to 50°C to dissolve, and keep warm half an hour. The temperature was lowered to 15°C, and the material was discharged by centrifugation to obtain 15 kg of crystals and 26 kg of filtrate.

[0044] to split

[0045] 3510 g of DL-pantoolactone, 60 g of methanol and 9 g of water were added to the mother liquor obtained in Example 1 to prepare a pantoolactone solution with a water content of 1.15% and a concentration of 90.9%, and the temperature was raised to 50° C. for dissolution. Under stirring conditions, add 410 g of 50-400 mesh L-(+)-pantolactone crystals to the above solution at 15°C as seed crystals, keep stirring at a temperature of 9-13°C, and use the same method as in Example 1. The optical rotation was monitored by the same method. After stirring...

Embodiment 3

[0047] Seed preparation

[0048] In 50 liters of pilot test kettles, 24 kilograms of filtrates prepared by seed crystals in drop into embodiment 1, 0.3 kilograms of sodium sulfate, 0.2 kilograms of water, 15.5 kilograms of D-(-)-pantolactones whose standard specific rotation is higher than 48.5 , start stirring, heat up to 85°C to dissolve, and keep warm for half an hour. Cool down to 15°C, centrifuge and discharge to obtain 15 kg of crystals and 25 kg of filtrate.

[0049] to split

[0050] Add 4993 g of DL-pantolactone and 80 ml of methanol to the mother liquor obtained in Example 2 to prepare a solution with a water content of 1.08% and a concentration of 91.3%, and heat up to 48° C. to dissolve. Under stirring conditions, add 416g of 50-400 mesh D-(-)-pantolactone crystals to the above solution at 13°C as seed crystals, maintain the temperature at 9-13°C, and use the same method as in Example 1 Monitor the optical rotation. After stirring for 4 hours, take a sample to d...

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Abstract

The invention discloses a process for preparing optically active pantoolactone by decomposing pantoolactone. In the process, firstly, a saline solution is used to prepare crystal seeds, and then alcohols or alcohol solutions are used as solvents to dissolve pantoate Lactone is made into a solution, under stirring and at a suitable temperature, add D‑(‑)‑pantoolactone crystals or L‑(+)‑pantoolactone crystals as seed crystals to stir and induce, and the system is stirred during stirring. Monitor the optical rotation. When the optical rotation does not exceed the specified value, cool down and stir. When the monitored optical rotation does not exceed the requirements, finally obtain the crystals by suction filtration, and recrystallize the crystals until the specific optical rotation meets the requirements, that is, the target product is obtained. The method of the invention avoids the defects of difficult recovery of resolution reagents in traditional industrial methods; avoids the defects of strong solvent toxicity, high solvent cost and unstable production in other induced resolution methods. The production process is relatively simple, the separation efficiency is high, and the mother liquor can be recycled, which greatly reduces the production cost.

Description

technical field [0001] The invention relates to a preparation method of optically active pantolactone, in particular to a new method for preparing optically active pantolactone by inducing splitting of pantolactone. Background technique [0002] The chemical name of D-pantolactone is α-hydroxy-β, β-dimethyl-γ-butyrolactone. As an important pharmaceutical intermediate, it is mainly used in the synthesis of vitamin drugs D-panthenol and Neurotrophic drug D-calcium pantothenate. Calcium D-pantothenate is vitamin B5, and as an important nutrient, it is widely used in feed additives, food additives, medicine and other fields; D-panthenol is provitamin B5, and is widely used in hair care products and cosmetics. [0003] The traditional industrial methods for preparing D-pantolactone are chemical resolution and biological resolution. These two methods have complex production processes, tedious preparation and recycling of resolution reagents, and high production costs; the patente...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
CPCC07D307/33C07B2200/07
Inventor 吴江
Owner 安徽泰格生物科技有限公司
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