Method for preparing o-hydroxybenzonitrile from methyl salicylate and urea

A technology for o-hydroxybenzonitrile and methyl salicylate, which is applied in the field of preparing o-hydroxybenzonitrile, can solve the problems of high cost of raw materials, short service life of catalysts, heavy environmental pollution, etc., and achieves low cost of raw materials and avoidance of oxidation. , the effect of a wide range of sources

Active Publication Date: 2020-05-12
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Technical problem solved: This application discloses a method for preparing o-hydroxybenzonitrile by using methyl salicylate and urea. The technical problem solved is that the existing In the o-hydroxybenzonitrile production technology, the raw material cost is high, the one-time investment is large, the service life of the catalyst is short, the use of non-essential excipients is large, the environment is polluted, and the use of highly toxic and toxic excipients is insufficient. The invention of the method for preparing o-hydroxybenzonitrile with methyl benzoate and urea promotes the clean production of o-hydroxybenzonitrile and the greening of the production process, promotes the efficient use of resources, and makes the production of o-hydroxybenzonitrile more in line with "Low emission, low pollution, low consumption, high safety" chemical production requirements

Method used

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  • Method for preparing o-hydroxybenzonitrile from methyl salicylate and urea
  • Method for preparing o-hydroxybenzonitrile from methyl salicylate and urea
  • Method for preparing o-hydroxybenzonitrile from methyl salicylate and urea

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Effect test

Embodiment 1

[0030] Such as figure 1 Shown, a kind of method utilizing methyl salicylate and urea to prepare o-hydroxybenzonitrile comprises the following steps:

[0031] The first step: artificial zeolite, silica gel, alumina, SiO 2 , ZrO 2 Or molecular sieves are weighed according to the ratio of its mass to phosphoric acid mass of 1.0:0.5~15.0, soaked in phosphoric acid aqueous solution with a mass percentage concentration of 10%~80% for 2.0~48.0 hours, then filtered to remove the liquid phase, and the obtained The solid matter is burned in a muffle furnace at 300°C-800°C for 2.0-24.0 hours, and then the solid material burned at high temperature is crushed to a particle size of 50-300 mesh to obtain the immobilized phosphoric acid catalyst;

[0032] Step 2: Weigh methyl salicylate and urea according to the mass ratio of methyl salicylate and urea as 1.0:1.0~6.0, and add methyl salicylate and urea into the reaction bottle;

[0033] Step 3: Install a stirring device, an ammonia gas int...

Embodiment 2

[0040] A preparation using methyl salicylate and urea figure 1 The method for the o-hydroxybenzonitrile of shown structure, comprises the following steps:

[0041] The first step: artificial zeolite, silica gel, alumina, SiO 2 , ZrO 2 Or molecular sieves are weighed according to the ratio of its mass to phosphoric acid mass of 1.0:0.5~15.0, soaked in phosphoric acid aqueous solution with a mass percentage concentration of 10%~80% for 2.0~48.0 hours, then filtered to remove the liquid phase, and the obtained The solid matter is burned in a muffle furnace at 300°C-800°C for 2.0-24.0 hours, and then the solid material burned at high temperature is crushed to a particle size of 50-300 mesh to obtain the immobilized phosphoric acid catalyst;

[0042] Step 2: Weigh methyl salicylate and urea according to the mass ratio of methyl salicylate and urea as 1.0:1.0~6.0, and add methyl salicylate and urea into the reaction bottle;

[0043] Step 3: Install a stirring device, an ammonia g...

Embodiment 3

[0049] A preparation using methyl salicylate and urea figure 1 The method for the o-hydroxybenzonitrile of shown structure, comprises the following steps:

[0050] The first step: artificial zeolite, silica gel, alumina, SiO 2 , ZrO 2 Or molecular sieves are weighed according to the ratio of its mass to phosphoric acid mass of 1.0:0.5~15.0, soaked in phosphoric acid aqueous solution with a mass percentage concentration of 10%~80% for 2.0~48.0 hours, then filtered to remove the liquid phase, and the obtained The solid matter is burned in a muffle furnace at 300°C-800°C for 2.0-24.0 hours, and then the solid material burned at high temperature is crushed to a particle size of 50-300 mesh to obtain the immobilized phosphoric acid catalyst;

[0051] Step 2: Weigh methyl salicylate and urea according to the mass ratio of methyl salicylate and urea as 1.0:1.0~6.0, and add methyl salicylate and urea into the reaction bottle;

[0052] Step 3: Install a stirring device, an ammonia g...

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Abstract

Methyl salicylate and urea are used as basic raw materials; artificial zeolite, silica gel, aluminum oxide, SiO2, ZrO2 or a molecular sieve and the like are soaked in a phosphoric acid aqueous solution and then fired at a high temperature to obtain immobilized phosphoric acid which takes the artificial zeolite, the silica gel, the aluminum oxide, the SiO2, the ZrO2 or the molecular sieve as a carrier, and the immobilized phosphoric acid is used as a catalyst to perform in-situ catalytic dehydration on methyl salicylate and salicylamide generated by a reaction of urea in an ammonia atmosphere at a high temperature; a mixed material containing o-hydroxybenzonitrile is directly prepared from methyl salicylate and urea; and finally, cooling and condensing are carried out step by step or the condensed mixed material containing the o-hydroxybenzonitrile is rectified to obtain an o-hydroxybenzonitrile product with the mass percentage content of more than 97% at the yield of more than 70% relative to the mass of the methyl salicylate.

Description

technical field [0001] The invention belongs to the field of fine organic chemicals in the field of organic synthesis, and relates to a method for preparing o-hydroxybenzonitrile by utilizing methyl salicylate and urea. Background technique [0002] o-Hydroxybenzonitrile, also known as 2-hydroxybenzonitrile, 2-cyanophenol, o-cyanophenol, salicylonitrile, CAS registration number is 611-20-1, is a kind of chemical with a melting point of 92~95℃ White crystalline solid. O-Hydroxybenzonitrile is an important intermediate in organic synthesis, and has important applications in the preparation of the medicine Bunirolol and the methoxyacrylate agricultural fungicide azoxystrobin. At the same time, o-hydroxybenzonitrile can also be used as an intermediate for the synthesis of various liquid crystal materials and spices. [0003] The synthesis methods of o-hydroxybenzonitrile mainly include the following types: (1) Salicylamide dehydrating agent dehydration method, which essentia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/53
CPCC07C253/20C07C231/10C07C255/53C07C235/60
Inventor 蔡照胜徐鹏王璇魏馨旖黄旭娟陈云王泳安吴桓瀚
Owner YANCHENG INST OF TECH
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