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Preparation method of octadecanedioic acid mono-tert-butyl ester-PFP

A technology of octadecanedioic acid and mono-tert-butyl ester, which is applied in the field of pharmaceutical preparation, can solve the problems of low purity, difficult coupling of tert-butyl ester, and unsuitability for popularization of production, and achieve simple post-processing and high reaction efficiency Effect

Pending Publication Date: 2021-10-01
浙江泽瑞生物医药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention provides a method for preparing octadecanedioic acid mono-tert-butyl ester-PFP, which can effectively solve the problem of octadecanedioic acid or octadecanedioic acid or octadecanedioic acid used in the preparation of polypeptide side chains such as semaglutide in the market. The coupling of tert-butyl ester of alkanedioic acid is difficult, the purity is low, and the problem that it cannot be suitable for popularization and production

Method used

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  • Preparation method of octadecanedioic acid mono-tert-butyl ester-PFP

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Embodiment 1

[0032] Such as figure 1 As shown, the present invention provides technical scheme, a kind of preparation method of mono-tert-butyl octadecanedioate-PFP,

[0033] Including the preparation of compound 1 and the preparation of mono-tert-butyl octadecanedioate-PFP;

[0034] Wherein the preparation of compound 1 comprises the following steps:

[0035]

[0036] S1. In the reaction kettle, add octadecanedioic acid, toluene, tert-butanol, start stirring, add (Boc) after heating 2 O reaction was stirred at room temperature overnight;

[0037] The reactor of S1 in compound 1 is 50L, the heating temperature is 70 degrees, and the reaction time is 4.5h;

[0038] S2, post-processing: 10L of reaction solution is decompressed and rotary evaporated to 5L, added DCM solution to dilute to 10L, washed with 10L of water, filtered and separated to keep the organic layer, then washed with 10L of 5% phosphoric acid aqueous solution and separated to keep the organic layer, Finally, wash the s...

Embodiment 2

[0055] Such as figure 1 As shown, the present invention provides technical scheme, a kind of preparation method of mono-tert-butyl octadecanedioate-PFP,

[0056] Including the preparation of compound 1 and the preparation of mono-tert-butyl octadecanedioate-PFP;

[0057] Wherein the preparation of compound 1 comprises the following steps:

[0058]

[0059] S1. In the reaction kettle, add octadecanedioic acid, toluene, tert-butanol, start stirring, add (Boc) after heating 2 O reaction was stirred at room temperature overnight;

[0060] S2, post-processing: 10L of reaction solution is decompressed and rotary evaporated to 5L, added DCM solution to dilute to 10L, washed with 10L of water, filtered and separated to keep the organic layer, then washed with 10L of 5% phosphoric acid aqueous solution and separated to keep the organic layer, Finally, wash the separated liquid with 10L saturated brine and keep the organic layer;

[0061]S3. The organic layer is decompressed and ...

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Abstract

The invention discloses a preparation method of octadecanedioic acid mono-tert-butyl ester-PFP. The preparation method comprises the steps of preparation of a compound 1 and preparation of octadecanedioic acid mono-tert-butyl ester-PFP; wherein the preparation method of the octadecanedioic acid mono-tert-butyl ester-PFP comprises the following steps: A1, adding a compound 1, pyridine and DMF into a reaction kettle, starting stirring for completely dissolving the components, dropwise adding trifluoroacetic acid pentafluorophenol ester, separating out a solid, and reacting the components; A2, post-treatment: carrying out suction filtration on the reaction liquid, collecting light yellow or white solids, carrying out DMF pulping and suction filtration, collecting products, and carrying out vacuum drying to obtain 1.4 Kg of products. Herein,the prepared compound 1 is simple in reaction and post-treatment and can also be directly used for preparing octadecanedioic acid mono-tert-butyl ester-PFP, and a solid generated in the reaction for preparing the octadecanedioic acid mono-tert-butyl ester-PFP is the product, and a high-purity product can be obtained only by simple pulping. The coupling difficulty of octadecanedioic acid or tert-butyl ester of octadecanedioic acid used for preparing side chains of polypeptides such as semaglutide and the like is relatively high, while the octadecanedioic acid mono-tert-butyl ester-PFP can react only by adding alkali, so that the reaction efficiency is high.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, in particular to a preparation method of mono-tert-butyl octadecanedioate-PFP. Background technique [0002] Octadecanedioic acid is an important class of chemical raw materials. It is a kind of long-chain dibasic acid. Long-chain dibasic acid has a very wide range of uses. Using long-chain dibasic acid as raw material can synthesize special nylon, high-grade spices, High-grade hot-melt adhesives, cold-resistant plasticizers, high-grade lubricating oils, high-grade antirust agents, high-grade paints and coatings, etc.; [0003] However, the coupling of octadecanedioic acid or tert-butyl octadecanedioic acid used in the preparation of semaglutide and other polypeptide side chains in the market is relatively difficult and has low purity, which is not suitable for popularization and production. Contents of the invention [0004] The present invention provides a method for preparing o...

Claims

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Application Information

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IPC IPC(8): C07C67/02C07C69/63
CPCC07C67/02C07C67/08C07C69/63
Inventor 张自超贾晨锐张静于洪远
Owner 浙江泽瑞生物医药有限公司
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