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Preparation method for ketal

A ketal, cedar alkanediol technology, applied in chemical recycling, organic chemistry, etc., can solve problems such as poor selectivity, low conversion rate, and three wastes

Active Publication Date: 2018-06-22
PAPANNA BEIJING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the low conversion rate of the method for preparing Ambrocenide in the prior art, poor selectivity, and the shortcomings of a large amount of three wastes, and replace the original polyphosphoric acid+ For the system of dimethoxypropane + ethylene glycol dimethyl ether, the conversion rate of the condensation reaction can reach more than 99%, the selectivity is more than 90%, the yield is increased to more than 95%, and the reaction time is shortened from 24 hours to 2 hours. ~8 hours

Method used

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  • Preparation method for ketal

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Effect test

Embodiment 1

[0037] Mix 10g (42 mmol) of cedaranediol, 0.41 g (4.2 mmol) of sulfamic acid, 100 ml of ethyl acetate, and 9.5 g (91 mmol) of dimethoxypropane, and stir the reaction solution at 20-25°C Reacted for 24 hours, the reaction solution was washed with water twice, each time with 50 milliliters of water, washed to neutrality, then the organic phase was concentrated to dryness, and then recrystallized with ethanol to obtain 11.1 g of white crystals, the yield was 95%, and the GC content = 99.0%, GC-MS: m / z=238[M]+. The aqueous phase containing the catalyst was separated with toluene to obtain 0.5 g of sulfamic acid, which can be directly used repeatedly.

Embodiment 2

[0039] Mix 10g (42 mmol) of cedaranediol, 0.41 g (4.2 mmol) of sulfamic acid, 100 ml of ethyl acetate, and 9.5 g (91 mmol) of dimethoxypropane, and the reaction solution is heated and refluxed for 76 to 78 ℃ for stirring and reacting for 3 hours, the reaction solution was washed twice with 50 milliliters of water each time until neutral, and then the organic phase was concentrated to dryness to obtain 11.1 g of white crystals with a yield of 95%, GC content=99.0%, GC - MS: m / z=238[M]+. The aqueous phase containing the catalyst was dehydrated with benzene to obtain 0.5 g of sulfamic acid, which can be directly used repeatedly.

Embodiment 3

[0041] With 10g (42 millimoles) cedaranediol, 0.41 grams (4.2 millimoles) sulfamic acid (the catalyst that embodiment 1 reclaims and obtains), ethyl acetate 100 milliliters, 9.5g (91 millimoles) dimethoxypropane Mix, react the reaction solution at 20-25°C for 24 hours with stirring, wash the reaction solution with water twice, each time with 50 ml of water until neutral, then concentrate the organic phase to dryness, and then recrystallize with ethanol to obtain 11.1 g of white crystals , yield 95%, GC content=99.0%, GC-MS: m / z=238[M]+. The aqueous phase containing the catalyst was separated with toluene to obtain 0.5 g of sulfamic acid, which can be directly used repeatedly.

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Abstract

The invention discloses a preparation method for a ketal. The method comprises the following steps: adding cedrane diol, a catalyst, ethyl acetate and dimethoxy propane according to a ratio, performing a full reaction, washing a reaction liquid by using water to neutrality, performing concentration on an organic phase to dryness, and performing recrystallization to obtain white crystals, so as toobtain the ketal, wherein the catalyst is sulfamic acid, glycine or a mixture of the sulfamic acid and the glycine. According to the method provided by the invention, through research of a synthesis method of Ambrocenide, people find that selection of a catalytic system is a key to affect the reaction effect; a system of the catalyst, the ethyl acetate and the dimethoxy propane is used, the conversion rate of the condensation reaction can reach 99% or more, and the yield can reach 95% or more; and the catalyst can be recycled, so that three waste (waste water, waste gas and solid waste) is reduced, resources are saved, and industrialized production is facilitated.

Description

technical field [0001] The invention relates to a preparation method of ketal, which belongs to the technical field of organic synthesis. Background technique [0002] Ambrocenide (CAS: 211299-54-6) developed by Symphony is a new type of artificial ambergris, which has a very strong ambergris woody aroma and a very long-lasting aroma. A small amount of use will bring a very plump aroma , can be widely used in hair care, fabric care, beauty skin care and perfume and other fields. [0003] [0004] At present, Ambrocenide is synthesized in EP857723A1 using natural cedrene as the starting material. After epoxidation, the epoxy is hydrolyzed into diol and then condensed with acetone in three steps. The one-step condensation of diol and acetone has a low conversion rate, poor selectivity, and a low yield of only 50%, and a large amount of waste acid will be produced, which pollutes the environment and is unfavorable for industrial production. In CN102134228A, the condensatio...

Claims

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Application Information

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IPC IPC(8): C07D317/70
CPCC07D317/70Y02P20/584
Inventor 张志虎程宾徐格赵雅楠管西艳
Owner PAPANNA BEIJING TECH
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