Synthetic method of p-nitroanisole

A technology of p-nitroanisole and synthetic method, which is applied in the field of synthesis of p-nitroanisole, can solve the problems of low yield of nitroanisole, and achieve the effect of improving yield

Pending Publication Date: 2021-03-12
ZHEJIANG HONGSHENG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem of low yield of p-nitroanisole in the preparation method of

Method used

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  • Synthetic method of p-nitroanisole

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Embodiment 1

[0039] refer to figure 1 , the present embodiment discloses a synthetic method of p-nitroanisole, which comprises the following steps:

[0040] S1: dissolved. In a 500mL three-neck flask, first add 70mL of organic solvent, the organic solvent is ethanol; then add reactant methanol 2.4mol. Then 0.48 mol of sodium hydroxide powder was added. Then use a mechanical stirrer to continuously stir; and install a condenser to condense and reflux. After observing that the sodium hydroxide is completely dissolved, the first mixed solution is formed.

[0041] S2: Initial response. Add 0.3 mol of p-nitrochlorobenzene into the three-necked flask where the first mixed solution is located, keep the reaction conditions and environment in step S1 and continue the reaction for 2.5 hours to obtain the second mixed solution.

[0042] S3: Secondary reaction. 0.512g of catalyst was added into the second mixed liquid, the catalyst was tetrapropylammonium bromide, and the reaction conditions and...

Embodiment 2

[0045] S1: dissolved. In a 500mL three-neck flask, first add 70mL of organic solvent, the organic solvent is ethanol; then add reactant methanol 2.4mol. Then 0.48 mol of sodium hydroxide powder was added. Then use a mechanical stirrer to continuously stir; and install a condenser to condense and reflux. After observing that the sodium hydroxide is completely dissolved, the first mixed solution is formed.

[0046] S2: Initial response. Add 0.3 mol of p-nitrochlorobenzene into the three-necked flask where the first mixed solution is located, keep the reaction conditions and environment in step S1 and continue the reaction for 2.5 hours to obtain the second mixed solution.

[0047]S3: Secondary reaction. Add 0.512g of catalyst into the second mixed liquid, choose tetrabutylammonium bromide as the catalyst, and keep the reaction conditions and environment of S1 for 6h.

[0048] S4: post-processing. The material in the three-necked flask after S3 treatment was directly filter...

Embodiment 3

[0050] S1: dissolved. In a 500mL three-neck flask, first add 70mL of organic solvent, the organic solvent is ethanol; then add reactant methanol 2.4mol. Then 0.48 mol of sodium hydroxide powder was added. Then use a mechanical stirrer to continuously stir; and install a condenser to condense and reflux. After observing that the sodium hydroxide is completely dissolved, the first mixed solution is formed.

[0051] S2: Initial response. Add 0.3 mol of p-nitrochlorobenzene into the three-necked flask where the first mixed solution is located, keep the reaction conditions and environment in step S1 and continue the reaction for 2.5 hours to obtain the second mixed solution.

[0052] S3: Secondary reaction. 0.512g of catalyst was added into the second mixed liquid, the catalyst was benzyltriethylammonium chloride, and the reaction conditions and environment of S1 were maintained for 6 hours.

[0053] S4: post-processing. The material in the three-necked flask after S3 treatme...

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Abstract

The invention relates to the technical field of organic intermediates, and particularly discloses a p-nitroanisole synthesis method. The method includes the steps: S1 dissolving p-nitroanisole, and dissolving sodium hydroxide and methanol in an organic solvent to form a first mixed solution, wherein the molar ratio of sodium hydroxide to methanol is (1.3-2): 8; S2, performing preliminary reaction,wherein p-nitrochlorobenzene is added into the first mixed solution for 2-3 h, and a second mixed solution is formed, and the molar ratio of the p-nitrochlorobenzene to the addition amount of the methanol in S1 is 1: 8; S3, carrying out secondary reaction: a catalyst is added into the second mixed solution, a quaternary ammonium salt catalyst is selected as the catalyst for 4-8 h, and the molar ratio of the addition amount of the catalyst to the addition amount of the methanol in S1 is (0.003-0.006): 8; S4, carrying out post-treatment, and carrying out post-treatment to obtain p-nitroanisole.By adding the quaternary ammonium salt catalyst, the final yield of p-nitroanisole can be improved.

Description

technical field [0001] The application relates to the technical field of organic intermediates, in particular to a synthetic method of p-nitroanisole. Background technique [0002] P-nitroanisole, also known as p-nitroanisole, is an intermediate for the synthesis of pesticides, medicines, organic dyes, pigments, etc. It is used to prepare a variety of pesticides, dyes, medicines, and food additives. It is a yellow shuttle at room temperature Crystal, which has a large demand in industry, is an important raw material for the synthesis of p-aminoanisole in industrial production. p-aminoanisole is widely used in the synthesis of spices, pesticides and rubber additives. [0003] In the related art, the production method of p-nitroanisole is to obtain p-nitrochlorobenzene through methoxylation under the action of a large amount of inorganic base. But there is the problem of low reaction yield in this process. Therefore, need badly to provide a kind of synthetic method of the hi...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C201/16C07C205/37
CPCC07C201/12C07C201/16
Inventor 张玉宝戴宽俊吴中礼鲁伟良
Owner ZHEJIANG HONGSHENG CHEM IND
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