Synthetic method of 2-(trimethylsilyl)-ethoxymethyl chloride

Abstract

The invention discloses a synthetic method of 2-(trimethylsilyl)-ethoxymethyl chloride. The reaction equation in the method is shown in the specification. According to the synthetic method of 2-(trimethylsilyl)-ethoxymethyl chloride disclosed by the invention, reactions are performed in normal pressure states and easy to control. Raw materials are products easily obtained massively in the market. The raw materials are low in cost and high in purity. Finally, reaction is performed in an alkaline condition, and the product is stable and long in retention time in the alkaline condition.

Description

technical field [0001] The invention relates to the technical field of organic synthesis methods suitable for large-scale industrial production, and specifically belongs to a synthesis method of 2-(trimethylsilyl)ethoxymethyl chloride. Background technique [0002] 2-(Trimethylsilyl)ethoxymethyl chloride (SEM-Cl) is a commonly used organosilicon protection reagent, and its functional selectivity is favored by many users. However, its high price, low product purity, and difficulty in preservation have always been problems that need to be solved urgently for this product. Prior Art The technical scheme generally adopted for this product is: the key intermediate of this product is trimethylsilyl ethanol, and then the final product SEM-Cl is obtained through chloromethylation reaction. There are two ways to synthesize the key intermediate trimethylsilyl ethanol at home and abroad: the first one: similar to the reformatsky reaction, under the action of active zinc powder, ethyl ...

AI Technical Summary

Problems solved by technology

[0008] Problems and shortcomings of existing technical solutions: the first synthetic method has been abandoned at home and abroad now, firstly the coupling yield of zinc powder participation in the first step is low, secondly the effect of using sodium borohydride during reduction is not ideal, lithium aluminum hydride The effect is good, but the risk of industrialization is high and the price is high

The second synthesis method is a method commonly used at home and abroad, but there are 2 points restricting its industrialization

The raw material price of its monochloromethyltrimethylsilane is high, which causes the price of the final product to be higher, which is a cost constraint to the downstream industry; secondly, when reacting with paraformaldehyde through the format method, due to the intense heat release, the current domestic and foreign Only about 2000L can be achieved, and the re-enlargement yield is low cost and high

Due to the involvement and selection of routes in the two synthetic methods, the price of raw materials and auxiliary materials is high, and the cost is passed on to the final product, resulting in high prices.

The last step of the two synthetic methods is chloromethylation. This reaction has many side reactions, and the purification of the final product is difficult. At present, domestic and foreign products can only achieve 95% content, and it is difficult to refine and expensive.

The final product is unstable under acidic conditions, and even if a stabilizer is added, the effect is not very satisfactory, and it is not convenient for long-term storage and use

Images