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Preparation method of [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide

A technology of dimethylamino and hydrobromide is applied in the field of preparation of [3-propyl]triphenylphosphonium bromide hydrobromide, which can solve the problem of reducing raw material cost, high reaction efficiency, reducing energy consumption, etc. To achieve the effect of reducing raw material cost, high reaction efficiency and reducing energy consumption

Inactive Publication Date: 2016-10-26
HUZHOU HENGYUAN BIOCHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on the technical problems existing in the background technology, the present invention aims at the problems of high cost, high energy consumption and low efficiency in the present preparation of [3-(dimethylamino)propyl] triphenylphosphine bromide hydrobromide, and provides A new preparation method of [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide, by optimizing the conditions of the process, directly use cheaper methanol as a solvent for normal temperature reaction, This reduces the cost of raw materials and energy consumption, and the reaction efficiency is high and the yield is high

Method used

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  • Preparation method of [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide
  • Preparation method of [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide

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Experimental program
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Effect test

Embodiment 1

[0021] Preparation of [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide

[0022]

[0023] Proceed as follows:

[0024] (1) Pump 200 kg of toluene into the reactor, manually add 90 kg of triphenylphosphine, quickly add 60 kg of 1,3-dibromopropane dropwise to the high tank, and reflux at 80°C for 5 hours at normal pressure. Cool, filter and dry to obtain white solid 3-bromopropyltriphenylphosphine bromide (P-I);

[0025] (2) Continue to pump 400 kg of methanol into the reaction kettle, manually add 150 kg of P-I into the methanol, and drop 100 kg of dimethylamine aqueous solution into the high level tank. After the addition, react at 50°C under normal pressure for 12 hours;

[0026] (3) After the reaction, methanol was evaporated to dryness under normal pressure, pumped into 400 kg of ethanol, heated to dissolve, cooled, filtered and dried to obtain white solid [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide Salt 211.5kg, yield 68.3%.

[00...

Embodiment 2

[0035] Preparation of [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide

[0036]

[0037] Proceed as follows:

[0038] (1) Pump 220 kg of toluene into the reactor, manually add 80 kg of triphenylphosphine, quickly add 70 kg of 1,3-dibromopropane dropwise to the high tank, and reflux for 6 hours under normal pressure at 80°C. Cool, filter and dry to obtain white solid 3-bromopropyltriphenylphosphine bromide (P-I);

[0039] (2) Continue to pump 420 kg of methanol into the reaction kettle, manually add 150 kg of P-I into the methanol, and drop 120 kg of dimethylamine aqueous solution into the high level tank. After the addition, the reaction was carried out at 50°C under normal pressure for 13 hours;

[0040] (3) After the reaction, methanol was evaporated to dryness under normal pressure, and 420 kg of ethanol was poured into the pump, heated to dissolve, then cooled, filtered and dried to obtain white solid [3-(dimethylamino)propyl]triphenylphosphine bromide...

Embodiment 3

[0044] Preparation of [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide

[0045]

[0046] Proceed as follows:

[0047] (1) Pump 180kg of toluene into the reaction kettle, manually add 100kg of triphenylphosphine, quickly drop 50kg of 1,3-dibromopropane into the high tank, reflux at 80°C for 6 hours at normal pressure, cool, filter and dry to obtain P-I ;

[0048] (2) Pump 350kg of methanol into the reaction kettle, manually add 150kg of P-I into the methanol, drop 80kg of dimethylamine aqueous solution into the high-level tank, and react for 14 hours under normal pressure at 50°C after the addition;

[0049] (3) After the reaction, the methanol was evaporated to dryness under normal pressure, and 390 kg of ethanol was poured into the pump, heated to dissolve, then cooled, filtered and dried to obtain a white solid [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide Salt 151.2kg, yield 62.7%.

[0050] Compared with the comparative test of Examp...

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Abstract

The invention discloses a preparation method of [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide. The preparation method is characterized by comprising the following steps: (1) 180-220 kg of toluene is pumped into a reaction kettle, 80-100 kg of triphenyl phosphine is added manually, 50-70 kg of 1,3-dibromopropane is added dropwise at a relatively high speed to an elevated tank, flux is performed for 5-6 h at normal pressure and at the temperature of 80 DEG C, and P-I is obtained through cooling, filtering and drying; (2) 350-420 kg of methanol is pumped into the reaction kettle, 150 kg of P-I is added to methanol manually, 80-120 kg of a dimethylamine aqueous solution is added dropwise to the elevated tank, and a reaction is performed for 10-14 h at normal pressure and at the temperature of 50 DEG C after addition; (3) methanol is evaporated to dryness after the reaction, 360-450 kg of ethanol is pumped in, cooling, filtering and drying are performed after heating for dissolution, and [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide is obtained.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to an improved preparation method of [3-(dimethylamino)propyl]triphenylphosphine bromide hydrobromide. Background technique [0002] Histamine is an active substance that exists in the body itself. It mainly forms complexes with polysaccharide sulfate, heparin or chondroitin sulfate and acidic proteins and exists in the granules of mast cells and basophils, especially in the lungs. , skin mucous membrane, bronchial mucous membrane, gastric mucosa and gastric parietal cells. When the tissue is stimulated by immune response or physical or chemical, it can cause mast cells to degranulate and release histamine, and the released histamine binds to histamine receptors, resulting in a pathophysiological response. Olopatadine hydrochloride is a safe and effective new type of histamine H1 receptor antagonist, which can highly selectively block the combination of histamine and H1 receptor, w...

Claims

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Application Information

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IPC IPC(8): C07F9/54
CPCC07F9/5407
Inventor 马维恒谢何青包建辉
Owner HUZHOU HENGYUAN BIOCHEM TECH
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