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A kind of preparation method of red base b

A red-based, reaction technology, applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, chemical instruments and methods, etc., can solve the problems of large amount and proportion of wastewater discharge, and achieve less wastewater discharge, small steric hindrance, The effect of less by-products

Active Publication Date: 2017-10-03
XIANGSHUI HENRYDA TECH CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The proportion of by-product bright red base RC is large by protecting amino groups with acetyl groups. About 172kg of red base RC is produced for every ton of red base B produced. Red base B accounts for 85.32%, and by-product bright red base accounts for 14.68%.

Method used

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  • A kind of preparation method of red base b
  • A kind of preparation method of red base b

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A clean preparation method for red base B, comprising the steps of:

[0037] (1) Preparation of o-carboxamido anisole: add 40g of anthranilate in a 500ml reaction vessel, add 350ml of toluene, add 20.9g of formic acid, start stirring, heat up to 100-102°C, and react for 3 hours , reclaim formic acid and toluene by distillation, add 300ml water to the residue, stir for 1 hour, leave standstill for 2 hours, filter to obtain o-carboxamide anisole, liquid chromatography analysis (area normalization method, the same below) product purity 96.13%, fold The hundred weight is 46.61g, and the yield is 95%.

[0038] (2) Preparation of 2-methoxy-4-nitrocarboxanilide: add 200ml of 98% concentrated sulfuric acid in a 500ml reaction vessel, start stirring, slowly add the o-carboxamidoanisole prepared in step (1), At a temperature of 35°C, slowly add 25.2 grams of 98% nitric acid dropwise, control the reaction temperature at 35-45°C, and the dropwise addition time is about 1.5 hours. ...

Embodiment 2

[0041] This example provides a clean preparation method for red base B, which is basically the same as Example 1. The difference is: in the first step in Example 1, 350ml of chlorobenzene was used as the solvent for the acylation reaction of o-formamide anisole, which was used to prepare o-formamide anisole, and o-formamide anisole was obtained. The product had a purity of 96.2%. The hundred weight is 46.72g, and the yield is 95.2%.

Embodiment 3

[0043] This example provides a clean preparation method for red base B, which is basically the same as Example 1. The difference is: the filtrate produced during the second step in Example 1 to prepare 2-methoxy-4-nitrocarboxanilide is denitrated and concentrated to a solution with a mass concentration of sulfuric acid of 89% and a solution with a mass concentration of 98%. Concentrated sulfuric acid is mixed in a volume ratio of 4:1 to form a mixed solution, which is used as a sulfuric acid solution for the preparation of 2-methoxy-4-nitroformanilide to obtain 2-methoxy-4 -Nitroformanilide was converted into 56.43g, and the yield was 93.4%.

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Abstract

The invention relates to a preparation method of red base B. In the presence of an acylation reaction solvent, o-aminoanisole and formic acid are subjected to formylation reaction at 80-102°C, and o-formamide is obtained by filtration after the reaction Anisole: o-formamide anisole is added to the sulfuric acid solution, and when the temperature of the reaction system is controlled at 0-70°C, nitric acid is added to the reaction system for nitration reaction, and after the reaction is completed, it is obtained by filtration 2-methoxy-4-nitroformanilide; 2-methoxy-4-nitroformanilide is hydrolyzed at 80~120°C in the presence of sulfuric acid and water. After the reaction, Separation, adjusting the pH to 6-7 with soda ash, and then filtering to obtain the red base B. The product of the invention has high yield, low cost, good quality and few by-products, greatly reduces the waste water produced in the production process of the red base B, meets the requirements of clean production, is easy to operate, and is convenient for industrialization.

Description

technical field [0001] The invention relates to a preparation method of fine chemical products, in particular to a preparation method of red base B. Background technique [0002] The red base B, whose structure is shown in formula I, is an important fine chemical intermediate, which is widely used in the organic pigment industry, such as for the manufacture of organic pigment yellow 74#, etc., and has a large market demand. [0003] [0004] Chinese patent CN200610013270.1 discloses a preparation method of red base B, put anisole, acetic anhydride and solvent dichloroethane into the reactor for acetylation reaction; and add fuming nitric acid dropwise in the reaction liquid, For nitration reaction; add sodium hydroxide for hydrolysis to remove acetyl. This method adopts acetic anhydride as protecting group, and the cost is higher, in addition to generating 2-methoxyl-4-nitroacetanilide during the nitration of o-acetamidoanisole, a high proportion of by-product 2-methoxyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/84C07C213/08
Inventor 张正富易元龙
Owner XIANGSHUI HENRYDA TECH CHEM
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