A kind of synthetic method of dye compound red base kd

A dye compound and synthesis method technology, applied in the field of dye compound synthesis, can solve the problems of long reaction process, long cycle, toxicity, etc., and achieve the effects of improving production efficiency, avoiding use and emission, and high yield

Active Publication Date: 2017-08-18
舟山欧莱克新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, there are many defects in this method, such as the raw material anisole has certain toxicity to the human body, the reaction process is long, and the cycle is long, etc.

Method used

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  • A kind of synthetic method of dye compound red base kd
  • A kind of synthetic method of dye compound red base kd
  • A kind of synthetic method of dye compound red base kd

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Its specific operation is as follows:

[0048] S1: at room temperature, add 100mmol of the following formula (I) compound 4-methoxy-3-aminobenzyl alcohol, 150mmol of the following formula (II) compound, 10mmol composite catalyst (for 5mmol 1-di A mixture of phenylphosphino-1'-(di-tert-butylphosphino)ferrocene and 5 mmol bis(cyclopentadienyl) zirconium dichloride), 120 mmol oxidant cerium ammonium nitrate and 8 mmol organic ligand L1, and then The temperature was raised to 80°C, and the reaction was stirred at this temperature for 10 hours;

[0049] S2: After the reaction of step S1 is completed, directly add 300 mmol of reducing agent Na 2 S (being the aqueous solution form of mass percent concentration 30%), and continue to react at 80 ℃ for 14 hours, after finishing, through aftertreatment, thereby obtain the following formula (III) compound (being red base KD) for white powder, The yield was 93.8%.

[0050] The specific reaction formula and process are as follows: ...

Embodiment 2

[0055] Its specific operation is as follows:

[0056] S1: at room temperature, add 100mmol of the formula (I) compound 4-methoxy-3-aminobenzyl alcohol, 250mmol of the formula (II) compound, 6mmol composite catalyst (3mmol 1 - a mixture of diphenylphosphino-1'-(di-tert-butylphosphino)ferrocene and 3 mmol bis(cyclopentadienyl) zirconium dichloride), 160 mmol oxidant cerium ammonium nitrate and 4 mmol organic ligand L1 , then warming up to 100°C, and stirring and reacting at this temperature for 6 hours;

[0057] S2: After the reaction in step S1 is completed, directly add 400 mmol of reducing agent NaHS (in the form of an aqueous solution with a mass percentage concentration of 50%), and continue to react at 100° C. for 10 hours, and after the end, undergo post-treatment to obtain a white powder The compound of formula (III) (ie the red base KD) has a yield of 93.5%.

[0058] The reaction formula and flow process as well as various characterization data are the same as in Exam...

Embodiment 3

[0060] Its specific operation is as follows:

[0061] S1: at room temperature, add 100mmol described formula (I) compound 4-methoxy-3-aminobenzyl alcohol, 200mmol described formula (II) compound, 8mmol composite catalyst (being 4mmol 1 - a mixture of diphenylphosphino-1'-(di-tert-butylphosphino)ferrocene and 4 mmol bis(cyclopentadienyl) zirconium dichloride), 140 mmol oxidant ceric ammonium nitrate and 6 mmol organic ligand L1 , then warming up to 90°C, and stirring and reacting at this temperature for 8 hours;

[0062] S2: After the reaction in step S1 is completed, directly add 350 mmol of reducing agent Na 2 S (in the form of an aqueous solution of 40% concentration by mass), and continued to react at 90°C for 12 hours, and after finishing, the compound of formula (III) was obtained as a white powder (i.e. the red base KD) , and the yield was 93.6%.

[0063] The reaction formula and flow process as well as various characterization data are the same as in Example 1, and w...

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Abstract

The invention relates to a synthesizing method of a dye compound 3-amino-4-methoxy benzanilide. The synthesizing method includes the steps of S1, in organic solvent and in the presence of composite catalyst, oxidizing agent and organic ligand, allowing a compound as shown in formula (I) and a compound as shown in formula (II) to react with each other; S2, directly adding reducing agent to perform reduction reaction after the reaction of the step S1, and performing post-treatment to obtain the 3-amino-4-methoxy benzanilide. The synthesizing method has the advantages that by using an appropriate reaction substrate and the comprehensive selection and coordination of the catalyst, the oxidizing agent, the organic ligand and the organic solvent, the 3-amino-4-methoxy benzanilide can be synthesized in a high-yield manner; in addition, the reaction flow is shortened, and the method is promising in application prospect and good in production potential.

Description

technical field [0001] The invention relates to a synthesis method of a dye compound, more particularly to a synthesis method of a red base KD, and belongs to the technical field of dye compound synthesis. Background technique [0002] In the field of dyes, the red base KD is a very important class of compounds. Its chemical name is 3-amino-4-methoxybenzamide, and its structural formula is as follows: [0003] [0004] Red-based KD is a new variety that has been put into production in my country in recent years. After diazotization, it can be dyed strong red on cotton thread and / or cotton cloth. It is mainly used for dyeing and printing of cotton-viscose and hemp fibers. In addition, the red base KD is also an important intermediate for the synthesis of other organic pigments, for example, it can be used to synthesize C.I. Pigment Red 31, 32, 146, 147, 150, 176, 261 and C.I. Pigment Violet 43. [0005] It is precisely because of such an important and wide application of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/00C07C231/02C07C231/12C07C237/44C07C235/56
CPCC07C231/00C07C231/02C07C231/12C07C235/56C07C237/44
Inventor 毛忠杰叶平龙杨淑清张仁坤
Owner 舟山欧莱克新材料科技有限公司
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