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Preparation method of permitil

A technology for preparing fluphenazine hydrochloride, which is applied in the field of preparation of fluphenazine hydrochloride, can solve problems such as increased production costs, substandard product quality, side reactions, etc. Good, the effect of reducing the difficulty of purification

Inactive Publication Date: 2015-12-16
JIANGSU BAOZONG & BAODA PHARMACHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past, there were side reactions in the production reaction process, the product quality was not up to standard, and the production cost was increased.

Method used

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  • Preparation method of permitil

Examples

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Effect test

Embodiment 1

[0012] (1) Preparation of 2-trifluoromethylphenothiazine: Add 100g (0.356mol) flufenamic acid into the reaction flask, heat to 180-190°C, start stirring, and add 10g into the reaction flask after it is completely melted (0.178mol) iron powder, stirred and reacted at 180-190°C for about 2 hours. After the reaction, when the reaction solution was cooled to 100°C, pour the reaction solution into the beaker while it was still hot, and the iron powder remained at the bottom of the reaction bottle (available water rinse). The reaction solution was added to a clean reaction flask and distilled under reduced pressure, and the fraction at 134-135°C (3mmHg) was collected to obtain about 67.5 g of light yellow liquid 3-trifluoromethyldiphenylamine, with a yield of about 80%.

[0013] Add 60g (0.253mol) of 3-trifluoromethyldiphenylamine and 8g (0.253mol) of sublimed sulfur into the reaction flask, heat up to about 130°C under stirring, add 3g of iodine to the reaction flask after the sulf...

Embodiment 2

[0018] (1) Preparation of 2-trifluoromethylphenothiazine: Add 500g (1.78mol) flufenamic acid into the reaction flask, heat to 180-190°C, start stirring, and add 50g into the reaction flask after it is completely melted (0.89mol) iron powder, stirred and reacted at 180-190°C for about 2 hours. After the reaction, when the reaction solution was cooled to 100°C, pour the reaction solution into the beaker while it was still hot, and the iron powder remained at the bottom of the reaction bottle (available water rinse). The reaction solution was added to a clean reaction flask and distilled under reduced pressure, and the fraction at 134-135°C (3mmHg) was collected to obtain about 346g of light yellow liquid 3-trifluoromethyldiphenylamine, with a yield of about 82%.

[0019] Add 300g (1.265mol) of 3-trifluoromethyldiphenylamine and 40g (1.265mol) of sublimed sulfur into the reaction flask, heat up to about 130°C under stirring, add 15g of iodine to the reaction flask after the sulfu...

Embodiment 3

[0024] (1) Preparation of 2-trifluoromethylphenothiazine: Add 1000g (3.56mol) flufenamic acid into the reaction flask, heat to 180-190°C, start stirring, and add 100g into the reaction flask after it is completely melted (1.78mol) iron powder, stirred and reacted at 180-190°C for about 2 hours. After the reaction, when the reaction solution was cooled to 100°C, pour the reaction solution into the beaker while it was still hot, and the iron powder remained at the bottom of the reaction bottle (available water rinse). The reaction solution was added to a clean reaction flask and distilled under reduced pressure, and the fraction at 134-135°C (3mmHg) was collected to obtain about 1029g of light yellow liquid 3-trifluoromethyldiphenylamine, with a yield of about 82%.

[0025] Add 600g (2.53mol) of 3-trifluoromethyldiphenylamine and 80g (2.53mol) of sublimed sulfur into the reaction flask, heat up to about 130°C under stirring, add 30g of iodine to the reaction flask after the sulf...

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Abstract

The invention discloses a preparation method of permitil. The preparation method is characterized by comprising the following steps: (1) taking flufenamic acid as a starting material, and carrying out decarboxylation and a cyclization reaction to prepare an intermediate 2-trifluoromethyl phenothiazine; (2) taking 1-(2-ethoxyl)piperazine, and 1,3-bromochloropropane as raw materials, carrying out a substitution reaction to prepare an intermediate 1-(3-chloropropyl)-4-(2-ethoxyl)piperazine; (3) carrying out a condensation reaction between the two intermediates to prepare an anatensol base, and salifying the anatensol base with hydrogen chloride gas to prepare the permitil. The preparation method is simple and convenient to operate, and free from risks and poisonous reactions; the prepared permitil is low in cost and high in purity.

Description

technical field [0001] The present invention relates to the preparation of fluphenazine hydrochloride and its intermediates, in particular to the use of catalyst iron powder during the preparation of the intermediate 2-trifluoromethylphenothiazine, and the feeding of 0.5 equivalent cyclizing agent during the cyclization reaction process +The application of raw material recovery process; the application of hydrogen chloride gas salt removal and purification process in the preparation of intermediate 1-(3-chloropropyl)-4-(2-hydroxyethyl)piperazine; It is the application of sodium hydroxide inorganic alkali fluoric acid agent + toluene reflux water separation process in the preparation of static hydrochloride. Background technique [0002] Fluphenazine hydrochloride, the chemical name is 4-[3-[2-(trifluoromethyl)-10H-phenothiazin-10-yl]propyl]-1-piperazineethanol dihydrochloride, It is clinically used as a drug for the treatment of mental illness. In the past, there will be s...

Claims

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Application Information

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IPC IPC(8): C07D279/28
CPCC07D279/28
Inventor 严家庆陈荣张智红
Owner JIANGSU BAOZONG & BAODA PHARMACHEM
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