Synthetic method of 1,4-dioxane-2,5-diol

Abstract

A synthetic method of 1,4-dioxane-2,5-diol is characterized in that concrete preparation comprises the following steps of: (1) feeding; (2) reacting; (3) post-processing; (4) preparation of the product. The invention has following advantages: 1, raw materials adopted in the invention are easily available and are cheap in price; the raw materials are all commercial raw materials or raw materials which are easy to prepare, and can satisfy the requirement of large scale production; 2, by the adoption of a simple hydrolysis reaction and simultaneously a batch charging method, the solvent amount is less, the energy and post-processing time are saved, the operation is simple, the synthetic method is suitable for large scale industrial production; 3, the condition of chemical reactions adopted in the invention is mild; there is no high temperature or low temperature reaction during the whole reaction process; during the production process, the technology is reasonable, the production is safe and reliable, and the cost is low; there is no environmental pollution; the synthetic method is suitable for large scale industrial production.

Description

(1) Technical field: [0001] The invention relates to a method for preparing a pharmaceutical intermediate, in particular to a method for synthesizing 1,4-dioxane-2,5-diol. (2) Background technology: [0002] 1,4-Dioxane-2,5-diol It is an important intermediate for the synthesis of various natural products, such as serine. Widely used in the production of medicines, pesticides, leather, rubber, preservatives, flavors and fragrances and dyes; used in high-purity metal surface treatment agents; important intermediates for pesticides and pharmaceutical chemicals, with important medicinal value and development prospect. [0003] At this stage, the methods for preparing this compound mainly include the following categories: [0004] (1) with As the starting material, water is used as the solvent, reacted under strong alkali and low temperature conditions, filtered, and distilled to obtain the target product. In this method, the amount of solvent is large, the post-treatment time is lo...

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Problems solved by technology

[0005] (2) to As a raw material, it is synthesized with deuterated acetonitrile in the presence of a photosensitizer. The reaction conditions are harsh, the raw material is expensive, and the cost is high. It is basically produced in the form of by-products and has no industrial application value. See references Miranda, Miguel A .; Izquierdo, M.Angeles; Perez-Ruiz, Raul; Journal of Physical Chemistry A: Molecules, Spectroscopy, Kinetics, Environment, & General Theory; vol.107; nb.14; (2003); p.2478-2482

[0006] (3) With 1,4-dioxane as the starting material, through three-step synthesis, the intermediate products are respectively This method has lengthy steps and complex operating procedures, so it is not suitable for large-scale production

[0007] (4) Taking benzyl bromide and ethylene glycol as starting materials, through 3-step synthesis, the intermediate product is This method requires the use of expensive Pd / C as a catalyst, and the reaction steps are longer, and the cost of the catalyst is relatively high

[0008] (5) Taking vinyl acetate as the starting material, through four-step synthesis, the intermediate products are respectively The steps of this method are lengthy and the scale-up production cost is high

[0009] The above synthetic methods are not suitable for large-scale production because of lengthy steps, complicated operation procedures and expensive raw materials.

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