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Method for preparing nor-tropine

A technology of nortropine alcohol and potassium hydroxide, which is applied in the new preparation field of nortropine alcohol, can solve the problems of difficulty in organic solvent extraction, increase the difficulty of extraction, and low solubility, so as to save consumption, reduce dosage, The effect of saving solvent

Active Publication Date: 2013-06-12
NINGBO TEAM PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] 2. Nortropine alcohol has good water solubility, but low solubility in organic solvents, so it is quite difficult to extract with organic solvents
[0008] 3. Potassium hydroxide and chloroform with high concentration are easy to generate diclocarbine, and careless operation may cause punching or even explosion
This further increases the difficulty of extraction

Method used

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  • Method for preparing nor-tropine

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Embodiment Construction

[0021] The following are preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto.

[0022] 1, in the autoclave of 1000 liters, draw in the potassium hydroxide aqueous solution (163kg (90%) potassium hydroxide adds 740kg water) that prepares. Then pump in 100kg of liquid N-ethoxycarbonylnortropine alcohol at about 70°C, stir and mix well, vacuumize, and then fill with nitrogen to 2-3kg / cm 2 , then stir and mix, vacuumize, and release nitrogen to 1kg / cm 2 .

[0023] Turn on the stirring, heat the steam to about 150°C, keep the heat for 1 hour, and gradually increase the pressure in the kettle to 8kg / cm 2 , open the vent valve to reduce the pressure to 4kg / cm 2 About 5 hours at 150°C for 5 hours, during which the pressure will rise to 5kg / cm 2 . After the reaction is complete, open the vent valve to reduce the pressure to normal pressure, pass circulating water to cool down to 60°C, and take a sample for testin...

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Abstract

The invention relates to a novel method for producing and preparing nor-tropine. The method comprises the following steps: taking N-alkoxycarbonyl nor-tropine as a raw material, adopting a small amount of potassium hydroxide (2-10 equivalent weights); rapidly hydrolyzing at the temperature of 100-160 DEG C and at high pressure of 1-10 atmospheric pressure and cooling to -5 to 10 DEG C after finishing reaction; filtering the collected and precipitated product; and carrying out recrystallization by ethyl acetate to obtain the product with purity being more than 99%. The products are all in extravert-type structure by GC detection. The method has the following advantages: 1. reducing the dosage of the potassium hydroxide to 10-25% of original dosage, thus saving the cost; 2. leaving out the cumbersome operation of chloroform and extraction, saving solvent, saving a large number of manpower and reducing pollution; 3. the actual pressure is about 5kg which is safe relatively when a high pressure autoclave is operated, thus eliminating explosion risk generated by the reaction of chloroform and potassium hydroxide; and 4. the color and luster and purity of the product is higher.

Description

technical field [0001] The invention relates to a new preparation method of nortropine alcohol, which belongs to the field of medicine and chemical industry. Background technique [0002] Nortropine alcohol, chemical name: 8-aza-bicyclo[3,2,1]octanol-2, as an important pharmaceutical intermediate, is used in the synthesis of many tropine alcohols. Its synthesis process is generally derived from the hydrolysis of N-alkoxycarbonyl nortropine alcohol. [0003] [0004] British Patent GB2184726 describes a method for preparing nortropine alcohol by hydrolyzing N-alkoxycarbonyl nortropine alcohol in potassium hydroxide solution. [0005] But the method described in this patent has many disadvantages: [0006] 1. A large amount of potassium hydroxide is used. In order to make the reaction have a faster speed, the amount of potassium hydroxide needs to reach more than 20 equivalents, and the concentration requires more than 20%. [0007] 2. Nortropine alcohol has good water ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D451/06
Inventor 费志刚张海诚黄道飞
Owner NINGBO TEAM PHARMA
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