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Preparation method of drug intermediate 2-aminonorbornane

A kind of technology of norbornane and borane

Inactive Publication Date: 2012-08-15
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method route for preparing 2-aminonorbornane hydrochloride is complicated and the yield is low

Method used

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  • Preparation method of drug intermediate 2-aminonorbornane
  • Preparation method of drug intermediate 2-aminonorbornane
  • Preparation method of drug intermediate 2-aminonorbornane

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 1) BH 3 · Preparation of THF (borane-tetrahydrofuran adduct)

[0019] Instrument reagent pretreatment:

[0020] All required glass instruments were dried at 110°C and assembled while hot, and cooled to room temperature under nitrogen protection.

[0021] bp: BF at 126℃ / 760mmHg 3 ·Et 2 O is processed as follows: per 500ml BF 3 ·Et 2 Add 2g CaH to O 2 and 10ml of anhydrous diethyl ether, distilled at 70°C under nitrogen protection to obtain a colorless and transparent solution, which should be stored away from light;

[0022] d = 0.9451, bp = 162°C, mp = -68°C Diglyme is treated as follows: CaH 2 Dry and store for 1-2 days until no bubbles overflow, and evaporate at 78°C under reduced pressure.

[0023] Under nitrogen protection, add 148.2g NaBH in the 2000ml three-neck flask in ice-water bath 4 and 1000ml Diglyme (diethylene glycol dimethyl ether), under nitrogen pressure, add BF dropwise through a double-ended needle 3 ·Et 2 O 630ml. Add 2000ml of d...

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Abstract

The invention relates to a preparation method of a drug intermediate 2-aminonorbornane, and belongs to the field of fine chemical engineering. In the method, norbornene is used as an initial raw material, and the method comprises the following steps: firstly enabling an organic solvent to react with a borane-tetrahydrofuran adduct at low temperature to prepare norborneol borane; then putting the norborneol borane into ammonia, and uniformly stirring and cooling; slowly dropwise adding a sodium hypochlorite solution, reacting for 6 to 10 hours at a temperature of 15-25 DEG C, and adding inorganic acid into the reaction system; and separating, alkalizing, cleaning, drying and concentrating to obtain the 2-aminonorbornane. The preparation method has the advantages of high reaction speed, high product yield, low production cost, industrial preparation applicability and the like.

Description

technical field [0001] The invention relates to a method for synthesizing important intermediates of pharmaceutical and chemical auxiliary agents, in particular to a method for preparing 2-aminonorbornane alkane. technical background [0002] 2-Aminonorbornane is a fine chemical with a wide range of uses, widely used in the fields of medicine, cosmetics, spices and chemical additives. The current method for preparing 2-aminonorbornane hydrochloride has complicated routes and low yields. Contents of the invention [0003] Based on the above technical background, the preparation method provided by the present invention aims to improve the synthesis route and production process of 2-aminonorbornane hydrochloride, reduce costs, increase product yield, improve safety, and enrich organic synthesis methodology. [0004] This program includes the following steps: [0005] The preparation method of 2-aminonorbornane, taking norbornene as a starting material, first reacts with bor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/38C07C209/00
Inventor 王晓季张建廷刘东旺吕常山陈曦孟玮
Owner JIANGXI SCI & TECH NORMAL UNIV
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