IES87000B2

IES87000B2 - Drug intermediates aluminium isopropoxide synthesis method

Info

Publication number: IES87000B2
Application number: IES20180100A
Authority: IE
Inventors: Peng Xiangliang
Original assignee: Chengdu Zhong Heng Hua Tie Tech Co Ltd
Priority date: 2018-04-03
Filing date: 2018-04-03
Publication date: 2019-05-01
Also published as: IES20180100A2

Abstract

Drug intermediates aluminium isopropoxide synthesis method, comprises the following steps: adding 3 mol alumina, 4-5 mol isopropanol solution to the reaction vessel, raising the temperature of the solution to 40-46°C, refluxing for 50-60 min, lowering the temperature of the solution to 10-15°C, and continuing the reaction until oxidation aluminum powder is completely dissolved and continues to be refluxed for 90-110 min, and distilled under reduced pressure, the fractions of 110-120 °C are collected, washed with methanol solution and washed with methylene chloride solution, and dehydrated with dehydrating agent to obtain the final product.

Description

Drug intermediates aluminium isopropoxide synthesis method FIELD OF THE INV ENTION The present invention relates to drug intermediates aluminium isopropoxide synthesis method.

GENERAL BACKGROUND Aluminum isopropoxide is mainly used for heterogeneous plant alcohol, testosterone, progesterone, and other hormones intermediates, is also one of the raw materials of aluminate coupling agent for dehydrating agent, catalyst and waterproof agent of raw materials. However, most of the existing synthetic methods are complicated and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method for further improving the quality and yield of the product and reducing the byproduct content, it has important economic significance.

SUMMARY The purpose of the present invention is to provide drug intermediates aluminium isopropoxide synthesis method, comprises the following steps: (i) adding 3 mol alumina, 4-5 mol isopropanol solution to the reaction vessel, raising the temperature of the solution to 40-46°C, refluxing for 50-60 min, lowering the temperature of the solution to 10-15°C, and continuing the reaction until oxidation aluminum powder is completely dissolved and continues to be refluxed for 90-110 min, and distilled under reduced pressure, the fractions of 110-120 °C are collected, washed with methanol solution and washed with methylene chloride solution, and dehydrated with dehydrating agent to obtain the final product; wherein, the isopropyl alcohol solution in the step (i) has a mass fraction of 60-65%, the pressure of vacuum distillation in the step (i) is 10-15kPa. the methanol solution in the step (i) has a mass fraction of 70-75%, the methylene chloride solution the step (i) has a mass fraction of 80-85%, and the dehydrating agent in the step (i) is any one of anhydrous sodium sulfate and anhydrous potassium carbonate.

Throughout the reaction process can be the following reaction formula: 6i.CI ί3),€_:ΗΟΗ ι A|,o3 --------► 2[(αΐΛ),ϋΗΟ]3Λ1 + 3H2O Advantage of the present invention is that: reducing intermediate links reaction, decreasing the reaction time and improving the reaction yield.

DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS The following examples with reference to specific embodiments of the present invention are further illustrated: Drug intermediates aluminium isopropoxide synthesis method.

Embodiment 1 The reaction vessel is added 3mol alumina, 4mol isopropanol solution with a mass fraction of 60%, the reaction temperature is increased to 40 °C, refluxed for 50 min, the temperature of the solution is reduced to 10°C, and the reaction is continued until the alumina powder is completely dissolved, continue to reflux for 90 min, vacuum distillation at lOkPa, collecting fraction of 110°C, washed with methanol solution with a mass fraction of 70%, and with dichloromethane solution with mass fraction of 80%, dehydrated with anhydrous sodium sulfate dehydrating agent to obtain the final product aluminium isopropoxide 538.56g, yield 88%.

Embodiment 2 The reaction vessel is added 3mol alumina, 4.5mol isopropanol solution with a mass fraction of 62%, the reaction temperature is increased to 43°C, refluxed for 55 min, the temperature of the solution is reduced to 12°C, the reaction was continued until the alumina powder was completely dissolved, continue refluxing for lOOmin, 12kPa vacuum distillation, collecting fraction of 115°C, washed with the methanol solution with a mass fraction of 72%, washed with the dichloro methane solution with a mass fraction of 82%, dehydrated with anhydrous potassium carbonate dehydrating agent to obtain the final product aluminium isopropoxide 563.04 G, yield 92%.

Embodiment 3 The reaction vessel is added 3 mol alumina, 5mol isopropanol solution with a mass fraction of 65%, the reaction temperature is increased to 46°C, refluxed for 60 min, the temperature of the solution is reduced to 15°C, the reaction is continued until the alumina powder was completely dissolved, refluxed for llOmin, 15kPa vacuum distillation, collecting fraction of 120°C, washed with mass fraction of 75% methanol solution, and with dichloromethane solution with mass fraction of 75%, dehydrated with anhydrous sodium sulfate dehydrating agent to obtain the final product aluminium isopropoxide 581 40g, yield 95%.

Claims

1. Drug intermediates aluminium isopropoxide synthesis method, comprises the following steps: (i) adding 3 mol alumina, 4-5 mol isopropanol solution to the reaction vessel, raising the temperature of the solution to 40-46°C, refluxing for 50-60 min, lowering the temperature of the solution to 10-15”C, and continuing the reaction until oxidation aluminum powder is completely dissolved and continues to be refluxed for 90-110 min, and distilled under reduced pressure, the fractions of 110-120 °C are collected, washed with methanol solution and washed with methylene chloride solution, and dehydrated with dehydrating agent to obtain the final product; wherein, the isopropyl alcohol solution in the step (i) has a mass fraction of 60-65%, the pressure of vacuum distillation in the step (i) is 10-15kPa, the methanol solution in the step (i) has a mass fraction of 70-75%.

2. Drug intermediates aluminium isopropoxide synthesis method according to claim 1 wherein the methylene chloride solution the step (i) has a mass fraction of 80-85%.

3. Drug intermediates aluminium isopropoxide synthesis method according to claim 1 wherein the dehydrating agent in the step (i) is any one of anhydrous sodium sulfate and anhydrous potassium carbonate.