Preparation method of 1, 2, 2, 6, 6-pentamethyl-4-piperidone

A technology of tetramethylpiperidone and piperidone, applied in the field of chemical synthesis, can solve the problems of difficult industrialization and high cost, and achieve the effect of increasing yield and reducing cost

Inactive Publication Date: 2020-04-03
宿迁联盛科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of its by-products are non-recyclable macromolecular impurities, and its cost is huge, so it is destined to be difficult to industrialize

Method used

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  • Preparation method of 1, 2, 2, 6, 6-pentamethyl-4-piperidone
  • Preparation method of 1, 2, 2, 6, 6-pentamethyl-4-piperidone
  • Preparation method of 1, 2, 2, 6, 6-pentamethyl-4-piperidone

Examples

Experimental program
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Effect test

Embodiment 1

[0026] In a 500ml four-neck flask equipped with a thermometer, add 155g of 2,2,6,6-tetramethylpiperidone, 300g of acetone, and 100g of sodium hydroxide, install a condenser, and slowly add 150g of dimethyl sulfate dropwise, And control temperature is 35 ℃. The dropwise addition was completed within 2 hours, and then the reaction was continued at this temperature for 5 hours. After cooling and filtering, the filtrate was concentrated and rectified to obtain the final product 1,2,2,6,6-pentamethyl-4-piperidone with a yield of 95%.

Embodiment 2

[0028] In a 500ml four-neck flask equipped with a thermometer, add 50g of 2,2,6,6-tetramethylpiperidone, 80g of acetonitrile, and 80g of sodium carbonate, install a condenser, slowly add 60g of dimethyl sulfate dropwise, and The control temperature is 45°C. The dropwise addition was completed within half an hour, and then the reaction was continued at this temperature for 3 hours. After cooling and filtering, the filtrate was concentrated and rectified to obtain the final product 1,2,2,6,6-pentamethyl-4-piperidone with a yield of 96%.

Embodiment 3

[0030] In a 500ml four-necked flask equipped with a thermometer, add 100g of 2,2,6,6-tetramethylpiperidone, 210g of DMF, and 200g of potassium carbonate, install a condenser, slowly add 120g of dimethyl sulfate dropwise, and control The temperature is 50°C. The dropwise addition was completed within 2 hours, and then the reaction was continued at this temperature for 4 hours. After cooling and filtering, the filtrate was concentrated and rectified to obtain the final product 1,2,2,6,6-pentamethyl-4-piperidone with a yield of 96.6%.

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Abstract

The invention discloses a preparation method of 1, 2, 2, 6, 6-pentamethyl-4-piperidone. The preparation method comprising following steps: taking 2, 2, 6, 6-tetramethylpiperidone as a raw material; inthe presence of an alkaline substance and in a solvent, stirring at a certain temperature and dropwise adding a certain amount of dimethyl sulfate for reaction, reacting for a certain period of timeafter the dropwise addition is finished, after the reaction is finished, cooling, filtering, concentrating and rectifying to obtain the final product 1, 2, 2, 6, 6-pentamethyl-4-piperidone. The yieldof the product can reach 95% or above, the yield is greatly increased, the cost is reduced, and the practical significance of industrialization can be achieved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of hindered amine light stabilizer intermediate 1,2,2,6,6-pentamethyl-4-piperidone. Background technique [0002] Hindered amine light stabilizer HALS is a high-performance light stabilizer developed on the basis of tetramethylpiperidone. In recent years, the development trend of hindered amine light stabilizers is mainly high molecular weight, low alkalinity, multifunctional, and polymerizable. Among them, the progress of low alkalinization, in recent years, mainly focuses on changing =NH, and alkylating =NH into =N-R, such as the light stabilizer GW-540 and BASF's Tinuvin 765, which all change the =NH on the piperidine group Methylated; or =NH alkoxylated =N-OR, such as BASF's Tinuvin 371, Tinuvin 123, thereby reducing its alkalinity and improving its acid resistance. [0003] 1,2,2,6,6-pentamethyl-4-piperidinol and 1,2,2,6,6-pentam...

Claims

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Application Information

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IPC IPC(8): C07D211/74
CPCC07D211/74
Inventor 袁开锋刘恩静胡新利项瞻峰
Owner 宿迁联盛科技股份有限公司
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