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A kind of method for preparing 2-chloro-4-isopropylpyridine

A technology of propylpyridine and hydroxyisopropyl, which is applied in the field of organic chemical synthesis, can solve the problems of low reaction conversion rate, expensive raw materials, and easy production of impurities, and achieve the effects of high product yield, high purity, and simple operation

Active Publication Date: 2022-04-19
SHANGHAI LINKCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] However, the reaction conversion rate in the existing synthesis technology is low, impurities are easily produced, and the raw materials are relatively expensive, which is not conducive to industrial production. Therefore, it is necessary to develop a new preparation method

Method used

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  • A kind of method for preparing 2-chloro-4-isopropylpyridine
  • A kind of method for preparing 2-chloro-4-isopropylpyridine
  • A kind of method for preparing 2-chloro-4-isopropylpyridine

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Experimental program
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Effect test

Embodiment 1

[0031] Step 1: Dissolve methyl 2-chloroisonicotinate (340g) in THF (6800ml) at room temperature, dissolve the system, lower the temperature and control the temperature at -50~-60°C, add dropwise 1M methylmagnesium bromide tetrahydrofuran solution (5000ml ), the dropwise addition is completed. Naturally warm up to room temperature (20-30°C) for 2 hours. After the reaction was completed, the temperature was lowered to 0-10°C, and the reaction was quenched by adding a saturated ammonium chloride solution dropwise, stirred for 0.5 h, left to stand and separated, the aqueous phase was extracted once with EA, and the combined organic phases were concentrated to dryness at 50°C. 322 g of light yellow oily liquid was obtained, with a yield of 95.3%.

[0032] Step 2: Add 4-(2-hydroxyisopropyl)-2-chloropyridine (400g), triethylsilane (1200g), trifluoroacetic acid (1340g) to the reaction flask, and heat up to (110-120°C) Reflux the reaction for 5 hours, the raw materials reacted comple...

Embodiment 2

[0035] Step 1: Dissolve methyl 2-chloroisonicotinate (340g) in THF (6800ml) at room temperature, dissolve the system, lower the temperature and control the temperature at -20~-30°C, add dropwise 1M methylmagnesium bromide tetrahydrofuran solution (5000ml ), the dropwise addition is completed. Naturally warm up to room temperature (20-30°C) for 2 hours. After the reaction was completed, the temperature was lowered to 0-10°C, and the reaction was quenched by adding a saturated ammonium chloride solution dropwise, stirred for 0.5 h, allowed to stand and separated, the aqueous phase was extracted once with EA, and the organic phase was concentrated to dryness at 50°C. 316 g of light yellow oily liquid was obtained, with a yield of 93.5%.

[0036] Step 2: Add 4-(2-hydroxyisopropyl)-2-chloropyridine (200g), triethylsilane (600g), trifluoroacetic acid (670g) to the reaction flask, and heat up to (100-110°C) Reflux reaction for 20h, the reaction of the raw material is complete, and ...

Embodiment 3

[0038] Step 1: Dissolve methyl 2-chloroisonicotinate (340g) in THF (8000ml) at room temperature, dissolve the system, lower the temperature and control the temperature at -50~-60°C, add dropwise 1M methylmagnesium bromide tetrahydrofuran solution (5000ml ), the dropwise addition is completed. Naturally warm up to room temperature (20-30°C) for 2 hours. After the reaction was completed, the temperature was lowered to 0-10° C., the reaction was quenched by adding a saturated ammonium chloride solution dropwise, stirred for 0.5 h, left standing to separate layers, and the organic phase was concentrated to dryness at 50° C. 312 g of light yellow oily liquid was obtained, with a yield of 92.3%.

[0039] Step 2: Add 4-(2-hydroxyisopropyl)-2-chloropyridine (400g), triethylsilane (1200g), trifluoroacetic acid (1340g) to the reaction flask, and heat up to (80-90°C) After 14 hours of reflux reaction, the reaction of the raw materials was complete, lower the temperature to 60°C, add 25...

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Abstract

The invention discloses a method for preparing 2-chloro-4-isopropylpyridine, belonging to the technical field of organic synthesis. The steps of the preparation method of the present invention are as follows: using 2-chloroisonicotinic acid methyl ester as a raw material, reacting with a Grignard reagent to generate 4-(2-hydroxyisopropyl)-2-chloropyridine; and then reacting with a reducing agent. 2-chloro-4-isopropylpyridine with high yield and high purity is prepared. The product of the invention has high yield and high purity, and the raw materials are easy to obtain, and the operation is simple, which is beneficial to industrialized production.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for preparing 2-chloro-4-isopropylpyridine. Background technique [0002] In recent years, organic light-emitting diodes (OLEDs) have attracted the attention of scientists due to their advantages such as self-illumination, wide viewing angle, and high contrast. At present, with the dual innovation of luminescent materials and device structures, highly efficient red and green devices have been successfully prepared. However, it is worth noting that the performance of OLEDs based on blue light emission still needs to be further improved. At present, it is generally believed that efficient blue-light emitting materials are one of the keys to obtain high-performance OLEDs. Patent US 10,340,467B2 discloses a highly efficient luminescent material, its structural formula is as follows: [0003] [0004] 2-Chloro-4-isopropylpyridine can be used as an important inte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 陆茜崔赛德李健新庞强
Owner SHANGHAI LINKCHEM TECH CO LTD
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