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Preparation method of N-methyl-pentylamine

A technology of methyl amylamine and n-amylamine, which is applied in the field of preparation of N-methyl amylamine, can solve the problems of long process route, influence on product promotion and application, low yield and the like, and achieves stable process and high yield. High, simple route effect

Inactive Publication Date: 2013-04-03
张家港市大伟助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, for the preparation of this compound, the process route is too long or the yield is too low, which affects the promotion and application of this product. It is urgent to find a preparation method with stable process, simple route and high yield.

Method used

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  • Preparation method of N-methyl-pentylamine
  • Preparation method of N-methyl-pentylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 100mL of anhydrous toluene, 57.8mL (0.5mol) of n-pentylamine and 66mL (0.65mol) of benzaldehyde into the reactor, heat and reflux for 30~40min; evaporate the solvent, cool the residue to 0~5℃, and keep the temperature condition Add 66.5mL (0.7mol) of dimethyl sulfate in anhydrous toluene (200mL), then heat to reflux for 20~25min, remove toluene and benzaldehyde under reduced pressure; cool the remaining solution to -5~0℃, add solid KOH, adjust pH=9.0, separate the amine layer, and distill under reduced pressure to obtain N-methylpentylamine (colorless transparent liquid, b.p.116-117°C, product purity 98.3%, yield 72.3%).

Embodiment 2

[0015] Add 120mL of anhydrous toluene, 57.8mL (0.5mol) of n-pentylamine and 71mL (0.9mol) of benzaldehyde into the reactor, heat and reflux for 30~40min; evaporate the solvent, cool the residue to 0~5℃, and keep the temperature condition Add 66.5mL (0.7mol) of dimethyl sulfate in anhydrous toluene (210mL), heat and reflux for 20~25min, remove toluene and benzaldehyde under reduced pressure; cool the remaining liquid to -5~0℃, add solid KOH, adjust pH=8.0, separate the amine layer, and distill under reduced pressure to obtain N-methylpentylamine (colorless transparent liquid, b.p.116-117°C, product purity 98.7%, yield 71.9%).

Embodiment 3

[0017] Add 150mL of anhydrous toluene, 57.8mL (0.5mol) of n-pentylamine and 76mL (0.75mol) of benzaldehyde into the reactor, heat and reflux for 30~40min; evaporate the solvent, cool the residue to 0~5℃, and keep the temperature condition Add 71mL (0.75mol) of dimethyl sulfate in anhydrous toluene (150mL), heat and reflux for 20~25min, remove toluene and benzaldehyde under reduced pressure; cool the remaining solution to -5~0℃, add solid KOH , adjust the pH=9.0, separate the amine layer, and distill under reduced pressure to obtain N-methylpentylamine (colorless transparent liquid, b.p.116-117°C, product purity 98.8%, yield 72.6%).

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Abstract

The invention discloses a preparation method of N-methyl-pentylamine, which comprises the following steps of: adding anhydrous methylbenzene, n-pentylamine and benzaldehyde in a reactor, heating to reflux for 30-40minutes; evaporating to remove a solvent, cooling a residue to 0-5 DEG C, adding an anhydrous methylbenzene solution of dimethyl sulfate under the condition that the temperature is preserved, heating to reflux for 20-25minutes, decompressing and removing methylbenzene and benzaldehyde; and cooling the left solution to -5-0 DEG C, adding solid KOH, regulating pH to be 8.0-9.0, separating out an amine layer, and distilling at reduced pressure to obtain N-methyl-pentylamine. The preparation method disclosed by the invention is simple, low in requirement of equipment, stable in process, simple in route, high in yield, easy to post-process in a preparation process, and easy to industrialize.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of N-methylpentylamine. Background technique [0002] N-methylpentylamine is an important intermediate for the synthesis of bisphosphonate drug ebendronic acid sodium, and the US patent synthesis adopts the catalytic hydrogenation method (the yield is only 49%). [0003] At present, for the preparation of this compound, the process route is too long or the yield is too low, which affects the promotion and application of this product. It is urgent to find a preparation method with stable process, simple route and high yield. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a preparation method of N-methylamylamine with stable process, simple route and high yield. [0005] For solving the problems of the technologies described above, the technical solution adopted in the present inventio...

Claims

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Application Information

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IPC IPC(8): C07C211/08C07C209/00
Inventor 龚卫良黄德周
Owner 张家港市大伟助剂有限公司
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