AU2018100363A4 - Drug intermediates aluminium isopropoxide synthesis method - Google Patents

Drug intermediates aluminium isopropoxide synthesis method Download PDF

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Publication number
AU2018100363A4
AU2018100363A4 AU2018100363A AU2018100363A AU2018100363A4 AU 2018100363 A4 AU2018100363 A4 AU 2018100363A4 AU 2018100363 A AU2018100363 A AU 2018100363A AU 2018100363 A AU2018100363 A AU 2018100363A AU 2018100363 A4 AU2018100363 A4 AU 2018100363A4
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AU
Australia
Prior art keywords
solution
synthesis method
aluminium isopropoxide
mass fraction
washed
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AU2018100363A
Inventor
xiangliang peng
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Chengdu Zhong Heng Hua Tie Technology Co Ltd
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Chengdu Zhong Heng Hua Tie Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/68—Preparation of metal alcoholates
    • C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Abstract Drug intermediates aluminium isopropoxide synthesis method, comprises the following steps: adding 3 mol alumina, 4-5 mol isopropanol solution to the reaction 5 vessel, raising the temperature of the solution to 40-460 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 10 solution, and dehydrated with dehydrating agent to obtain the final product.

Description

FIELD OF THE INVENTION
The present invention relates to drug intermediates aluminium isopropoxide 5 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.
2018100363 24 Mar 2018
Throughout the reaction process can be the following reaction formula: 6(CfIi)2CI[OIl + Al20j -► 2L(CH3),CHOJ3A1 + 3H2U
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 dichloromethane 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%.
2018100363 24 Mar 2018
Embodiment 3
The reaction vessel is added 3mol 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%.
2018100363 24 Mar 2018

Claims (3)

  1. 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, 5 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
    10 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%.
    15
  2. 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. 3. Drug intermediates aluminium isopropoxide synthesis method according to
    20 claim 1 wherein the dehydrating agent in the step (i) is any one of anhydrous sodium sulfate and anhydrous potassium carbonate.
AU2018100363A 2017-02-07 2018-03-24 Drug intermediates aluminium isopropoxide synthesis method Ceased AU2018100363A4 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CN201710067489.8A CN108395366A (en) 2017-02-07 2017-02-07 A kind of synthetic method of pharmaceutical intermediate aluminium isopropoxide
GBGB1705311.7A GB201705311D0 (en) 2017-02-07 2017-04-03 Drug intermediates aluminium isopropoxide synthesis method
GBGB1705311.7 2017-04-03

Publications (1)

Publication Number Publication Date
AU2018100363A4 true AU2018100363A4 (en) 2018-05-10

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AU2018100363A Ceased AU2018100363A4 (en) 2017-02-07 2018-03-24 Drug intermediates aluminium isopropoxide synthesis method

Country Status (3)

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CN (1) CN108395366A (en)
AU (1) AU2018100363A4 (en)
GB (1) GB201705311D0 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113248345A (en) * 2021-06-11 2021-08-13 江苏华盛锂电材料股份有限公司 Preparation method of 2-butenol

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113248345A (en) * 2021-06-11 2021-08-13 江苏华盛锂电材料股份有限公司 Preparation method of 2-butenol
CN113248345B (en) * 2021-06-11 2021-10-26 江苏华盛锂电材料股份有限公司 Preparation method of 2-butenol

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Publication number Publication date
CN108395366A (en) 2018-08-14
GB201705311D0 (en) 2017-05-17

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