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CN-122010705-A - Synthesis method of Bojie Hong Quan

CN122010705ACN 122010705 ACN122010705 ACN 122010705ACN-122010705-A

Abstract

The invention relates to the technical field of organic compound synthesis, and discloses a synthesis method of a boscalid Hong Quan, which takes 4-tertiary butyl styrene as a raw material to prepare boscalid Hong Quan through a one-step hydroformylation reaction. Rh (CO) 2 C 5 H 7 O 2 and bis (2, 4-dicumylphenyl) pentaerythritol diphosphite form a composite catalyst, and the composite catalyst is matched with triethylamine organic base to react under specific process conditions, and then the pure product is obtained through reduced pressure rectification. The method has the advantages of simple process, mild reaction conditions, over 98 percent of raw material conversion rate, over 80 percent of product yield, over 98 percent of purity, easy recovery of reagents and small environmental hazard, and is suitable for industrial mass production.

Inventors

  • WANG BOGUO
  • ZHAO ZUOYI
  • XU KEWEN
  • HU FADONG
  • CHEN YONG
  • GAO MING

Assignees

  • 绵阳市斯麦尔顾生物科技有限公司

Dates

Publication Date
20260512
Application Date
20260205

Claims (7)

  1. 1. A synthesis method of a wave cleaner Hong Quan is characterized in that 4-tertiary butyl styrene is used as a raw material, wave cleaner Hong Quan is prepared through a one-step hydroformylation reaction, and the method specifically comprises the following steps: Step 1, adding a rhodium catalyst and a phosphine ligand into a polytetrafluoroethylene lining of a high-pressure reaction kettle, and uniformly stirring to obtain a catalyst system, wherein the rhodium catalyst is Rh (CO) 2 C 5 H 7 O 2 , and the phosphine ligand is bis (2, 4-dicumylphenyl) pentaerythritol diphosphite; Step 2, sequentially adding 4-tert-butylstyrene, solvent dimethylformamide and an organic alkali compound into the liner in the step 1, covering a kettle cover of a reaction kettle, and obtaining a closed reaction system after nitrogen leakage detection, nitrogen replacement and synthesis gas replacement, wherein the organic alkali compound is triethylamine, and the synthesis gas is hydrogen and carbon monoxide mixed gas with the volume ratio of 1:1; step 3, introducing synthesis gas into the reaction system in the step 2 until the pressure is 2.8-3.2 MPa, keeping constant, and cooling and decompressing after the reaction is finished at the stirring speed of 750-850 r/min and the temperature rising reaction time of 5-7 h to obtain a reaction product system; and 4, rectifying the reaction product system in the step 3 under reduced pressure to obtain a pure product of the Bojie Hong Quan.
  2. 2. The method for synthesizing the polishing Hong Quan according to claim 1, wherein in the step 1, the mass ratio of the rhodium catalyst to the phosphine ligand is 1 (8.0-8.2).
  3. 3. The method for synthesizing the boscalid Hong Quan according to claim 1, wherein in the step 2, the volume ratio of 4-tert-butylstyrene to dimethylformamide is 1:5.
  4. 4. The method for synthesizing the spray-dried powder Hong Quan according to claim 1, wherein in the step 2, the mass ratio of the 4-tert-butylstyrene to the triethylamine is 100 (0.8-0.9).
  5. 5. The method for synthesizing the corrugated Hong Quan according to claim 1, wherein in the step 3, the reaction temperature is 115-125 ℃.
  6. 6. The method for synthesizing the corrugated Hong Quan according to claim 1, wherein in the step 4, the pressure of the reduced pressure rectification is 0.08-0.09 mpa.
  7. 7. The method for synthesizing the corrugated Hong Quan according to claim 1, wherein in the step 4, the temperature of the vacuum rectification is 80-90 ℃.

Description

Synthesis method of Bojie Hong Quan Technical Field The invention relates to the technical field of organic compound synthesis, in particular to a synthesis method of a Bojie Hong Quan. Background The chemical name of the boscalid Hong Quan is 4- (1, 1-dimethylethyl) phenylpropionaldehyde, which is an important aromatic aldehyde compound and is widely applied to the fields of synthesis of perfumes, medical intermediates and fine chemical products. Its unique molecular structure imparts its excellent chemical activity and organoleptic properties, and plays an important role in high-end perfume formulations. At present, the synthesis method of the boscalid Hong Quan in the prior art is mainly a condensation method, and generally comprises three core steps of condensation reaction, hydrogenation reaction and hydrolysis reaction, namely, firstly, raw material aldehyde is subjected to condensation reaction to prepare an enal intermediate, then hydrogenation reduction is carried out under the action of a palladium-carbon catalyst, and finally, the boscalid formaldehyde product is obtained through hydrolysis reaction. However, the synthetic route has the technical defects of firstly complicated reaction steps, long process flow and low production efficiency caused by multi-step reaction, secondly obvious influence on product quality due to the selection of raw material aldehyde types, easy product purity fluctuation caused by different batches of raw materials, high difficulty in reaction process control, thirdly, more harmful environmental protection caused by partial reagents due to the use of various organic solvents and catalysts in the reaction process, and high difficulty in subsequent separation and purification, and high production cost, fourthly, the product yield of the traditional condensation method is generally low, the resource waste is serious, and the industrial large-scale production is not facilitated. Aiming at the defects of the existing condensation method, the field needs to develop a method for synthesizing the boscalid Hong Quan, which has the advantages of simple steps, low production cost, environmental friendliness and higher yield and purity. Disclosure of Invention In order to overcome the defects of the prior art, the invention aims to provide a synthesis method of the bose Hong Quan, which takes 4-tertiary butyl styrene as a raw material, directly prepares the bose Hong Quan through one-step hydroformylation reaction, has the advantages of simple process, high raw material conversion rate, high product yield, small environmental hazard and the like, and is suitable for industrial mass production. In order to achieve the purpose, the invention provides the following technical scheme that the synthesis method of the corrugated-clean Hong Quan takes 4-tertiary butyl styrene as a raw material, prepares the corrugated-clean Hong Quan through one-step hydroformylation, and specifically comprises the following steps: Step 1, adding a rhodium catalyst and a phosphine ligand into a polytetrafluoroethylene lining of a high-pressure reaction kettle, and uniformly stirring to obtain a catalyst system, wherein the rhodium catalyst is Rh (CO) 2C5H7O2, and the phosphine ligand is bis (2, 4-dicumylphenyl) pentaerythritol diphosphite; Step 2, sequentially adding 4-tert-butylstyrene, solvent dimethylformamide and an organic alkali compound into the liner in the step 1, covering a kettle cover of a reaction kettle, and obtaining a closed reaction system after nitrogen leakage detection, nitrogen replacement and synthesis gas replacement, wherein the organic alkali compound is triethylamine, and the synthesis gas is hydrogen and carbon monoxide mixed gas with the volume ratio of 1:1; step 3, introducing synthesis gas into the reaction system in the step 2 until the pressure is 2.8-3.2 MPa, keeping constant, and cooling and decompressing after the reaction is finished at the stirring speed of 750-850 r/min and the temperature rising reaction time of 5-7 h to obtain a reaction product system; and 4, rectifying the reaction product system in the step 3 under reduced pressure to obtain a pure product of the Bojie Hong Quan. Further, in the step 1, the mass ratio of the rhodium catalyst to the phosphine ligand is 1 (8.0-8.2). Further, in the step 2, the volume ratio of the 4-tertiary butyl styrene to the dimethylformamide is 1:5. Further, in the step 2, the mass ratio of the 4-tert-butylstyrene to the triethylamine is 100 (0.8-0.9). Further, in the step 3, the reaction temperature is 115-125 ℃. Further, in the step 4, the pressure of the reduced pressure rectification is 0.08-0.09 MPa. Further, in the step 4, the temperature of the reduced pressure rectification is 80-90 ℃. Compared with the prior art, the invention has the following beneficial technical effects: 1. The invention takes 4-tertiary butyl styrene as a raw material, directly prepares the boscalid Hong Quan through one-step hydroformylation react