Preparation method for red base B

A red-based, methoxy-based 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 of wastewater discharge and large proportion, and achieve less wastewater discharge and steric hindrance. Small, less by-product effect

Active Publication Date: 2015-11-18
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 i

Method used

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  • Preparation method for red base B
  • Preparation method for 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 for a red base B. A formylation reaction is performed on o-aminoanisole and formic acid at 80-102 DEG C on the condition that acylation reaction solvent exists, and filtration is performed to obtain o-formamide anisole after the formylation reaction is completed; the o-formamide anisole is added into a sulfuric acid solution, nitric acid is added into a reaction system to perform a nitration reaction when the temperature of the reaction system is controlled at 0-70 DEG C, and filtration is performed to obtain methoxyl-4-nitroformanilide after the nitration reaction is completed; a hydrolysis reaction is performed on the methoxyl-4-nitroformanilide on the condition that the sulfuric acid and water exist at 80-120 DEG C, after the hydrolysis reaction is completed, separation is performed, the pH value is regulated to 6-7 with sodium carbonate, and then filtration is performed to obtain the red base B. According to the preparation method, the produce yield is high, the cost is low, the quality is good, by-products are less, waste water generated in the production process of the red base B is greatly reduced, the clean production requirement is met, operation is easy and convenient, and industrialization is facilitated.

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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IPC IPC(8): C07C217/84C07C213/08
Inventor 张正富易元龙
Owner XIANGSHUI HENRYDA TECH CHEM
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