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Method for preparing methylamino hexahydropyridine

The technology of methylaminopiperidine and methylamino alcohol is applied in the field of preparation of 3-methylaminopiperidine, which can solve the problems of many by-products, difficult separation and purification, incomplete reaction and the like, achieves improved yield, simplified process operation, low cost effect

Inactive Publication Date: 2007-11-14
亚邦化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] This route has shortcomings such as incomplete reaction, many by-products, and difficulty in separation and purification.

Method used

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  • Method for preparing methylamino hexahydropyridine
  • Method for preparing methylamino hexahydropyridine
  • Method for preparing methylamino hexahydropyridine

Examples

Experimental program
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Effect test

Embodiment 1

[0043] 1, the preparation of 3-methylaminopyridine (B)

[0044] (1) Add 250g (1.49mol) of 3-bromopyridine, 1200ml (12mol) of methylamine aqueous solution (30%) and 24.1g (0.1mol) of copper sulfate in a 2L autoclave, heat to 200°C, pressure 4MPa, constant temperature After 12 hours, cool and discharge, concentrate the reaction solution under reduced pressure, add 200ml of 40% sodium hydroxide solution, extract with 1000ml of dichloromethane in 3 times, dry over anhydrous sodium sulfate, and recover the solvent. The residue was distilled under reduced pressure, and the fraction at 133-134°C (15 mmHg) was collected to obtain 142 g of a colorless oily liquid, with a yield of 88.4%.

[0045] (2) Add 250g (1.49mol) of 3-bromopyridine and 1200ml (12mol) of methylamine solution (30%) into a 2L autoclave, heat to 200°C, pressure 4MPa, keep constant temperature for 12h, cool and discharge, concentrate under reduced pressure After the reaction solution, 200 ml of 40% sodium hydroxide so...

Embodiment 2

[0048] 2, Preparation of 3-methylaminopiperidine

[0049] In a 2L autoclave, add 108g (1mol) of 3-methylaminopyridine (B), add 40g of Pd / C catalyst, 1200ml of ethanol, carry out the reduction reaction at 120°C and 20MPa for 24h, filter out the catalyst after cooling, and recover the filtrate solvent. Concentrate under reduced pressure, add dichloromethane to dissolve, wash twice with water, separate the water phase, and dry the organic phase with anhydrous sodium sulfate. Atmospheric distillation removed dichloromethane, added petroleum ether, crystallized, filtered, and dried to obtain 8.5 g of white solid with a yield of 78%.

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Abstract

This invention relates to the preparation method of 3 -methylamino- piperidine which is key intermediate of broad spectrum antibiosis type balofloxacin. The invention takes 3 - halogenated pyridine as raw material, takes catalytic ammoniation and catalytic reduction to gain product.

Description

technical field [0001] The invention relates to a preparation method of a key intermediate 3-methylaminopiperidine of a novel broad-spectrum antibacterial drug baloxacin. Background technique [0002] The official chemical name of baloxacin is 1-cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-7-(3-methylamino-1-piperidinyl)-4- Oxo-3-quinoline carboxylic acid, whose English name is balofloxacin, is a transformational broad-spectrum antibacterial drug jointly developed by Chugai Pharmaceutical Co., Ltd. of Japan and Choongwae Company of Korea. It was first launched in Korea in March 2002. This product is against G + and G - And anaerobic bacteria have a broad-spectrum antibacterial effect, and have strong antibacterial activity against Streptococcus pneumoniae, Klebsiella pneumoniae, Mycoplasma pneumoniae, Bacillus cloacae, and Haemophilus influenzae. It is mainly used clinically for sensitive respiratory tract, digestive tract, and urinary tract. and bone and soft tissue infect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/56
Inventor 石卫兵颜文革郭彦彰张虹
Owner 亚邦化工集团有限公司
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