Preparation method of 1, 2-di (o-amino phenoxyl) ethane

Abstract

The invention provides a preparation method of 1, 2-di (o-amino phenoxyl) ethane, belonging to the technical field of a compound preparation method, in particular to a preparation method of a fine chemical industrial midbody. The preparation method is characterized by sequentially comprising the two steps of: condensing o-nitro chlorobenzene with glycol under the existence of sodium carbonate, sodium hydroxide and phase transfer catalyst to prepare 1, 2-(o-nitro phenoxyl) ethane; and reducing the 1, 2-(o-nitro phenoxyl) ethane in organic solvent with hydrazine hydrate to prepare the 1, 2-di (o-amino phenoxyl) ethane. The yield of the two steps is obviously higher than that of the other document reports, and the purity of the product is higher than 99%. The method not only has low cost, but also has stable yield quality, thereby being a synthesis method which can be completely realized in the industrial production. The catalyst has low price and high yield; and the organic solvent is carbinol or alcohol, and has low price. The method nearly has no three wastes.

Description

technical field [0001] The invention belongs to the technical field of compound preparation methods, and in particular relates to a preparation method of a fine chemical intermediate. Background technique [0002] 1,2-bis(o-aminophenoxy)-ethane is a valuable fine chemical intermediate, in addition to being used in the synthesis of C.I. organic pigment yellow 180, it is also used in many dyes, paints, medicines, oils It is an important intermediate for product additives and Schiff base macrocycles. In the late 1990s, with the continuous expansion of the application field of 1,2-bis(o-aminophenoxy)-ethane terminal fine chemical products, especially Pigment Yellow 180, many domestic scientific research institutions focused on the development and research of this product also became active. But so far, the research results in this area generally have defects such as high cost, poor application performance of the product, and harsh conditions of the synthesis process, making it...

AI Technical Summary

Problems solved by technology

[0004] In order to obtain 1,2-bis(o-aminophenoxy)ethane, 1,2-bis(o-nitrophenoxy)ethane must be reduced. Foreign literature reports that the hydrazine hydrate route is basically Pd / C Or metal catalytic reduction methods such as Ruan's nickel, domestic related articles have reported that the product adopts the iron-carbon reduction route, and "Chemical Reagents" 199517 (1) 49-50 reported the same route as ours, but the report said The yield that can be achieved is only 86%, which has a large gap compared with the yield of this patent