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Production technology of pharmaceutical grade valeryl chloride

A technology of n-valeryl chloride and production technology, applied in the field of production technology of pharmaceutical-grade n-valeryl chloride, can solve problems such as only satisfying

Inactive Publication Date: 2015-06-24
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the 126-127°C fraction collected by rectification in this system has a purity of ≥98% (GC), and the content of n-valeric anhydride is about 1%, which only meets the pesticide-grade product index, and 5-10% of the black residue at the bottom of the rectification tank tar

Method used

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  • Production technology of pharmaceutical grade valeryl chloride
  • Production technology of pharmaceutical grade valeryl chloride
  • Production technology of pharmaceutical grade valeryl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 100kg of n-valeric acid and 140kg of thionyl chloride into the 500L enamel reaction kettle through the metering pump respectively from the storage tank, then add 0.1kg of DMF, open the steam valve, and raise the temperature to 50°C, the generated acid gas is discharged from the tail gas absorption device Absorb and react until no gas is released. Vacuum suck the above reaction solution into a 200L rectification kettle, add 0.1kg N,N-dimethylaniline, rectify under reduced pressure, control the temperature of the kettle to ≤90°C, recover 23kg of thionyl chloride, and collect 115kg of n-pentanoyl chloride. 99.7% (GC), yield 98%.

Embodiment 2

[0021] Put 100kg of n-valeric acid and 175kg of thionyl chloride into the 500L enamel reaction kettle through the metering pump respectively from the storage tank, then add 0.2kg of DMF, open the steam valve, raise the temperature to 70°C, and remove the generated acid gas to the tail gas absorption device Absorb and react until no gas is released. Vacuum suck the above reaction solution into a 200L rectification kettle, add 0.5kg of triphenylamine, rectify under reduced pressure, control the temperature of the kettle to be ≤90°C, recover 57kg of thionyl chloride, and collect 113kg of n-valeryl chloride with a purity of 99.6% (GC). The yield is 96%.

Embodiment 3

[0023] Put 100kg of n-valeric acid and 152kg of thionyl chloride into the 500L enamel reaction kettle through the metering pump respectively from the storage tank, then add 0.5kg of DMF, open the steam valve, raise the temperature to 90°C, and remove the generated acid gas to the tail gas absorption device Absorb and react until no gas is released. Vacuum the above reaction solution into a 200L rectification kettle, add 0.3kg of triethanolamine, rectify under reduced pressure, control the temperature of the kettle to ≤90°C, recover 35kg of thionyl chloride, and collect 114kg of n-pentanoyl chloride with a purity of 99.7% (GC). The yield is 97%.

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Abstract

The invention discloses a production technology of pharmaceutical grade valeryl chloride, relating to the field of chemical industry production. The production technology disclosed herein comprises the following steps: respectively pumping n-valeric acid and thionyl chloride into an enamel reaction kettle from storage tanks by using a metering pump, wherein the ratio of n(n-valeric acid) to n(thionyl chloride) is 1.0:1.2-1.0:1.5; then measured as n-valeric acid, adding 1-5wt% of DMF, heating up to 50-90 DEG C to react until no gas is generated; sucking the chlorination reaction liquid into a rectifying still under vacuum condition, measured as n-valeric acid, adding 1-5wt% of stabilizer, conducting rectification under vacuum, controlling the temperature of the rectifying still being no higher than 90 DEG C, collecting the front cut fraction thionyl chloride into a receiving storage tank, and collecting valeryl chloride into a finished product storage tank. According to the invention, by adding the electron-rich stabilizer to allow acyl cations to preferentially be combined with the stabilizer, thus the generation of valeric anhydride is avoided; simultaneously the temperature of the rectifying still is reduced, the equilibrium constant of valeryl chloride dissociation is reduced, and the stability of distillation separation is raised.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a production process of pharmaceutical grade n-valeryl chloride. Background technique [0002] N-valeryl chloride is a chemical product with a wide range of uses, such as the synthesis of pesticide fungicide hexaconazole; nematic phenylcyclohexane liquid crystal material; antihypertensive drugs perindopril, valsartan, irbeza Tan; and group protection in the field of organic synthesis, etc. Among them, pharmaceutical-grade n-valeryl chloride has high added value and the most stringent quality indicators, requiring n-valeryl chloride content ≥ 99.5%, n-valeric anhydride content ≤ 0.2%, n-valeric acid content ≤ 0.25%, and no phosphorus residues. [0003] The production method of n-valeryl chloride is to use n-valeric acid as the raw material and synthesize it by chlorination with chlorinating reagents. The optional chlorinating reagents include phosgene, thionyl chloride, phospho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/42C07C51/60C07C51/64
Inventor 方永勤褚俊轩武安邦许亮
Owner CHANGZHOU UNIV