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A kind of preparation method of dye intermediate

A technology of dye intermediates and cyanoacetyl, which is applied in the field of preparation of dye intermediates, can solve the problems of low product yield and low production yield, and achieve the effect of high product purity

Active Publication Date: 2022-04-15
杭州布朗生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the existing dye intermediate 2-(1-ethylpentane)-7-methyl-6 cyano-5-carbonyl-8,8-dihydro[1,2,4]triazolo[1 , 5-a] pyridine exists under the preparation yield, the problem that overall product yield is lower, the invention provides a kind of preparation method of dye intermediate

Method used

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  • A kind of preparation method of dye intermediate
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  • A kind of preparation method of dye intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Preparation of N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine:

[0054] Add 250g of hydrazine hydrate with a purity of 80wt% to a 2000mL flask, drop the temperature to 20°C, add 440g of methyl cyanoacetate dropwise, add 1800g of water after 2 hours of reaction, stir evenly, transfer to a 5L four-neck flask, add 400g of baking soda, 800g 1,4-dioxane, 5g PEG; cool down to 5°C, then add 710g isooctanoyl chloride dropwise, keep warm for 4 hours after the addition, discharge and filter, wash with water until neutral, and dry to obtain 880g N-cyanoacetyl Base-N'-(2-ethylhexanoyl)hydrazine, the calculated product yield is about 97.65%.

Embodiment 2

[0056] Preparation of N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine:

[0057] Add 250g of hydrazine hydrate with a purity of 80wt% to a 2000mL flask, drop the temperature to 5°C and add 460g of methyl cyanoacetate dropwise, add 2000g of water after 2 hours of reaction, stir evenly, transfer to a 5L four-necked flask, add 450g of sodium carbonate, 150g ethyl acetate, 5g TBAB; cool down to 15°C, then add 780g isooctanoyl chloride dropwise, keep warm for 4 hours after the addition, discharge and filter, wash with water until neutral, and dry to obtain 850g N-cyanoacetyl-N '-(2-Ethylhexanoyl)hydrazine, the calculated product yield is about 94.44%.

[0058] It can be seen from the above examples 1 and 2 that the technical solution for the preparation of N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine of the present invention can achieve efficient and high-yield preparation.

[0059] And the results of the orthogonal experiment based on Example 1 show that when the other parameters excep...

Embodiment 3

[0069] Dye intermediate 2-(1-ethylpentane)-7-methyl-6 cyano-5-carbonyl-8,8-dihydro[1,2,4]triazolo[1,5-a ] The preparation of pyridine: take 3-aminocrotononitrile and N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine as raw materials, place them in a mixed organic solvent and heat to reflux, carry out heating and reflux treatment A, and heat to reflux After treatment A, cool down to ≤110°C, add 0.65 times the weight of N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine anhydrous zinc chloride, and then heat and reflux treatment B, heat and reflux treatment After the end of B, cool down to ≤90°C, add 1.0 times the weight of N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine industrial concentrated hydrochloric acid, and evaporate to dryness to obtain 2-(1-ethylpentane )-7-methyl-6cyano-5-carbonyl-8,8-dihydro[1,2,4]triazolo[1,5-a]pyridine.

[0070] The specific parameters of this embodiment are shown in the table below.

[0071]

[0072] In the table: material A and material B respectively refe...

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Abstract

The invention belongs to the field of organic compounds, in particular to a preparation method of a dye intermediate. The method comprises: using 3-aminocrotononitrile and N-cyanoacetyl-N'-(2-ethylhexanoyl)hydrazine as raw materials, placing them in a mixed organic solvent and heating to reflux, and adding dehydration during the heating and reflux process Catalyst, add non-oxidative acid after heating and reflux, and evaporate to dryness to obtain dye intermediate. The method of the invention can carry out reflux reaction at high temperature, so that the yield of the product is greatly increased to more than 80%, and the purity of the product can still basically reach the purity of more than 98%.

Description

technical field [0001] The invention belongs to the field of organic compounds, in particular to a preparation method of a dye intermediate. Background technique [0002] In dyeing, coloring and toning techniques, 2-(1-ethylpentane)-7-methyl-6cyano-5-carbonyl-8,8-dihydro[1,2,4]triazine Azolo[1,5-a]pyridine is an important dye intermediate substance, which can be widely used in the fields of colored photosensitive resin materials, and the oily photosensitive resin composition can be used to manufacture color filters, liquid crystal displays, etc. Devices or solid-state image sensors and other fields. Therefore, as a dye intermediate substance, 2-(1-ethylpentane)-7-methyl-6cyano-5-carbonyl-8,8-dihydro[1,2,4]triazole And[1,5-a]pyridine has extremely high application value. [0003] At present, there is no special process research for this dye intermediate in China, and the existing patented technology for the preparation process of this dye intermediate is mainly in the hand...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 马肖克黄国祥
Owner 杭州布朗生物医药科技有限公司