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Preparation method of 3-methyl-2-cyclopentene-1-one

A technology of cyclopentene and methyl, which is applied in the field of preparation of 3-methyl-2-cyclopenten-1-one, can solve the problems of high energy consumption and safety risks, harsh conditions, etc., to reduce energy consumption, The effect of reducing pollution

Active Publication Date: 2020-12-04
LAVIANA TAIZHOU PHARMACHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in order to achieve the state of subcritical and supercritical water, the reaction needs to be carried out at a temperature of 300-400°C and a pressure of 9-40MPa, which is very harsh and requires high energy consumption and safety risks.

Method used

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  • Preparation method of 3-methyl-2-cyclopentene-1-one
  • Preparation method of 3-methyl-2-cyclopentene-1-one

Examples

Experimental program
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Effect test

Embodiment 1-1

[0029] Add deionized water (300 mL, 2.5 vol) to 2,5-hexanedione (120.0 g), stir well, and record it as solution A. Add deionized water (400 mL) to sodium hydroxide (100.0 g), stir well, and record it as solution B (ie 20% aqueous sodium hydroxide solution). Install the coil reactor, place it in an oil bath, and raise the external temperature to 125°C. Immerse the suction nozzles of plunger pump 1 (hereinafter referred to as pump 1) and plunger pump 2 (hereinafter referred to as pump 2) under the liquid surface of solution A and solution B respectively. Set the flow rate of pump 1 and pump 2 to 12.0mL / min, turn on the two pumps at the same time, and inject solution A and solution B into the reactor from the two feed ports of the reactor for reaction. The effluent from the outlet of the reactor was collected into a 250mL four-necked bottle, and cooled in an external bath at 0-5°C. After receiving the reaction solution for 5 minutes, the reaction was stopped and a sample was ta...

Embodiment 1-2

[0031] Add deionized water (222 mL, 1.85 vol) to 2,5-hexanedione (120.0 g, 1.0 eq), stir well, and record it as solution A. Other conditions are the same as in Example 1-1. After receiving the reaction solution for 5 minutes, the reaction was stopped and a sample was taken, and extracted with ethyl acetate for GC analysis. The molar ratio of sodium hydroxide to 2,5-hexanedione is 1.7:1.

Embodiment 1-3

[0033] Add deionized water (138 mL, 1.15 vol) to 2,5-hexanedione (120.0 g, 1.0 eq), stir well, and record it as solution A. Other conditions are the same as in Example 1-1. After receiving the reaction solution for 5 minutes, the reaction was stopped and a sample was taken, and extracted with ethyl acetate for GC analysis. The molar ratio of sodium hydroxide to 2,5-hexanedione is 1.3:1.

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Abstract

The invention provides a preparation method of 3-methyl-2-cyclopentene-1-one. A device comprises a coiled tube type reactor and two plunger pumps, the output ends of the plunger pumps are connected with the coiled tube type reactor, and the coiled tube type reactor is placed in an oil bath pan at 120-130 DEG C. The preparation method comprises the following steps: S1, preparing a 2, 5-hexanedioneaqueous solution and a 20% sodium hydroxide solution; S2, respectively immersing the plunger pumps into the 2, 5-hexanedione aqueous solution and the 20% sodium hydroxide solution, and setting the flow rate to be 10-18 mL / min; and S3, placing a 1 L four-necked bottle at the outlet of the reactor, cooling with heat-conducting oil at the temperature of 0-5 DEG C in an external bath, stopping the reaction and sampling after receiving the reaction liquid for 30 minutes, extracting with acetic acid, and carrying out GC analysis. According to the invention, a continuous reaction technology is adopted, and the reaction selectivity is regulated by adjusting the molar ratio, the feeding rate and the residence time of materials; and the reaction solution is collected and cooled after the reaction isfinished, thereby avoiding the quick decomposition of the product in the hot alkali liquor. Water is used as a solvent, and reaction is carried out at a low temperature, so environmental pollution isreduced, and energy consumption is reduced. And the yield of the prepared 3-methyl-2-cyclopentene-1-one reaches 70-75%.

Description

technical field [0001] The invention relates to a preparation method of 3-methyl-2-cyclopenten-1-one. Background technique [0002] 3-Methyl-2-cyclopenten-1-one is a light yellow to yellow-brown transparent liquid with a sweet caramel aroma. It can be used as spices and pharmaceutical intermediates, and can synthesize a variety of medicinal substances, including trichothecenes, adrenal cortex and so on. 3-Methyl-2-cyclopenten-1-one is also the precursor of various substituted cyclopentadiene, which can react with various metals to form metallocene complexes, such substances are alkenes An important class of catalysts for polymerization. In addition, 3-methyl-2-cyclopenten-1-one can also be used as a gasoline additive in the petrochemical industry, such as methylcyclopentane that can be generated after hydrogenation, which has a high octane number and Energy density, can be used as a good substitute for ethanol gasoline. [0003] Robinson et al. first use 2,5-hexanedione ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C49/597B01J19/00
CPCC07C45/74B01J19/0093B01J19/0006C07C2601/10C07C49/597
Inventor 朱耿宇
Owner LAVIANA TAIZHOU PHARMACHEM
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