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Production method of medicinal laurocapram

The invention relates to a technology of lauro azone and a production method, which are applied in the production of lauro azone and the production field of high-purity lauro azone, and can solve the problems of long production time, large amount of alkali used, etc., and achieve less environmental pollution and less reaction The effect of moderate temperature and simple production operation

Active Publication Date: 2014-12-24
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The technical problem to be solved in the present invention is that in the existing laurocaprazine production technology, the amount of alkali used is relatively large, and the production time is long, and a kind of technology three wastes is less, and the production of pharmaceutical grade laurocaprazine with high product purity is proposed production method

Method used

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  • Production method of medicinal laurocapram

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Effect test

preparation example Construction

[0029] Preparation of Solid Superbase Catalyst

[0030] Weigh KOH solid 28.1g, KF solid 29.1g, Al 2 o 3 Put 104.0g of fine powder into the reaction kettle, add 300mL of ethanol, turn on mechanical stirring, raise the temperature to 75°C, reflux for 1h, distill off the solvent under reduced pressure, put the solid in an oven, dry and activate at 115°C for 3h, and obtain KF-KOH / Al 2 o 3 Solid super base.

Embodiment 1

[0032] Weigh caprolactam 11.3g (0.1mol), KF-KOH / Al 2 o 3 Put 20.0g of catalyst into a stirred and heated reactor, add 100mL of cyclohexane solvent, raise the temperature to 45°C, stir for 1h, then add 27.4g of bromododecane, and 0.90g of KI solid, heat up to 70~75°C and reflux Reaction 1h. The reaction solution was filtered, and the filter residue was washed with an appropriate amount of cyclohexane until the identification reaction of laurocapram did not appear. The filtrate and cleaning solution were combined, and washed with saturated saline until the washing solution was close to neutral. After evaporating the solvent and rectifying under reduced pressure, collecting the fraction at 158-160°C under a vacuum of 0.66kPa to obtain 27.2 g of laurocapram, the content of laurocapram was >99.5%, and the yield was 93.9%.

Embodiment 2

[0034] Weigh caprolactam 56.5g (0.5mol), KF-KOH / Al 2 o 3 Put 100.0g of catalyst into a stirred and heated reactor, add 500mL of cyclohexane solvent, raise the temperature to 45°C, stir for 1.5h, then add 137.1g of bromododecane, and 4.5g of KI solid, and raise the temperature to 70~75°C Reflux reaction for 1.5h. The reaction solution was filtered, and the filter residue was washed with an appropriate amount of cyclohexane until the identification reaction of laurocapram did not appear. The filtrate and cleaning solution were combined, and washed with saturated saline until the washing solution was close to neutral. After evaporating the solvent and rectifying under reduced pressure, collecting the fraction at 158-160°C under a vacuum of 0.66kPa to obtain 129.6g of laurocaprazine, the content of laurocaprazine was >99.5%, and the yield was 94.2%.

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Abstract

The invention relates to a production method of medicinal laurocapram, which comprises the steps of adding bromo-n-dodecane, caprolactam, a solid super basic catalyst and a cocatalyst into a reactor in a certain proportion, adding an appropriate solvent, heating, preserving heat, performing reflux reaction, filtering and recycling the catalyst, washing an organic solution with a saturated saline solution, heating, distilling, removing water, then reducing pressure for rectification, and collecting a finished product of laurocapram.

Description

technical field [0001] The invention relates to the field of production technology, in particular to a production method of high-purity laurocapram, and is especially suitable for the production of pharmaceutical-grade laurocapram. Background technique [0002] Laurocaprazine, also known as laurocaprazine, has a chemical name of 1-dodecylazepan-2-one, and its chemical structural formula is as follows: [0003] [0004] The substance is a colorless and transparent viscous liquid, almost odorless and tasteless, and has good solubility in various organic solvents, specifically, in absolute ethanol, ethyl acetate, ether, benzene and cyclohexane Easily soluble but insoluble in water, it is a non-ionic surfactant. The substance has low toxicity, oral LD50>7g / kg, can improve skin cutin, promote cutin softening, and enhance its permeability. Transparency effect, widely used. [0005] The synthetic method of laurocaprolactone is various, and caprolactam and bromododecane ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10
CPCY02P20/584
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA
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