METHOD FOR PRODUCING ESTER BASED ON ECO-FRIENDLY AND HIGH-EFFICIENCY ESTERIFICATION BY USING BASE EXCHANGE OF SALT AND THE COMPOUND THEREOF

    公开(公告)号:US20230265039A1

    公开(公告)日:2023-08-24

    申请号:US17107037

    申请日:2020-11-24

    摘要: Provided are an environmentally-friendly high-efficiency method of manufacturing an ester compound based on an esterification reaction using a salt ion-exchange method and an ester compound manufactured thereby. In the conventional esterification reaction, an ester was produced in low yields due to the hydrolysis (i.e., reverse reaction) caused by water, or it was required to continuously supply hydrochloric acid gas or use thionyl chloride, which is a hazardous material, and thus there were limitations in terms of environmental friendliness or cost. On the other hand, in the present invention, hydrochloric acid gas is continuously supplied using the salt ion-exchange method, and since magnesium sulfate acts as a dehydrating agent, the water generated in the esterification reaction is removed, and thus the occurrence of hydrolysis (i.e., reverse reaction) is suppressed and a conversion rate to the desired ester compound is increased. In addition, since the reactants are inexpensive and the product is less hazardous and easy to handle, a more efficient reaction is possible.

    Method for producing tri-carbobenzoxy-arginine

    公开(公告)号:US10202337B2

    公开(公告)日:2019-02-12

    申请号:US15129927

    申请日:2015-03-23

    IPC分类号: C07C277/08

    摘要: A tri-carbobenzoxy-arginine represented by the following formula (2): is produced by carbobenzoxylating the arginine or arginine derivative (1) represented by the following formula (1), or a salt thereof: by adding carbobenzoxy chloride and a base in a water/organic solvent bilayer system to an arginine or arginine derivative (1) represented by the formula (1), or a salt thereof.

    AZD9291 intermediate and preparation method therefor

    公开(公告)号:US10167275B2

    公开(公告)日:2019-01-01

    申请号:US15822060

    申请日:2017-11-24

    发明人: Xuenong Xu

    摘要: Disclosed are an intermediate, N-[2-[[2-(dimethylamino)ethyl]methylamino]-4-methoxy-5-formamidine]phenyl-2-propenamide (II), applicable in preparing AZD9291 (I) and a preparation method for the intermediate. Preparation steps of the preparation method comprise: 2-fluoro-4-methoxyaniline, serving as a starting material, undergoes amidation, substitution, nitrification, reduction and guanidination reactions to prepare N-[2-[[2-(dimethylamino)ethyl]methylamino]-4-methoxy-5-formamidine]phenyl-2-propenamide (II). Also disclosed is a method for preparing AZD9291 (I) by means of a cyclization reaction between the compound of a formula II and (2E)-3-dimethylamino-1-(1-methyl-1H-indol-3-yl)-2-propen-1-one (III). The preparation method has readily available raw materials and a simple process and is economical, environmentally friendly, and suitable for industrialized production.