Method for preparing hexamethylbenzene by taking 2-butyne as raw material

A technology for hexatoluene and butyne, applied in the field of preparing hexatoluene, can solve the problems of high requirements on reaction conditions, waste of raw materials, and high energy consumption, and achieve the effects of less chemical raw materials, less by-products, and high energy consumption

Inactive Publication Date: 2015-01-28
SHANGHAI CHENGYING NEW MATERIALS
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Problems solved by technology

The traditional production method not only requires high reaction conditions and high energy co...

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  • Method for preparing hexamethylbenzene by taking 2-butyne as raw material
  • Method for preparing hexamethylbenzene by taking 2-butyne as raw material
  • Method for preparing hexamethylbenzene by taking 2-butyne as raw material

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Embodiment 1-11

[0023] The following examples relate to a method for preparing hexamethylbenzene with 2-butyne as a raw material, comprising the following steps: adding solvent and 2-butyne sequentially in a three-necked flask according to the ratio of raw materials, and then adding a required amount of palladium chloride catalyst and copper chloride co-catalyst, turn on the low-temperature cooling water circulation of the condenser (provided by a low-temperature tank, the coolant is a mixture of ethylene glycol-water, the temperature is -10°C), immerse the flask in a preheated oil bath, and turn on the magnetic force Stir and time to maintain the desired reaction temperature until complete. The product was cooled and filtered to remove the catalyst.

[0024] The composition of the reaction solution was obtained by gas chromatography analysis (see hexamethylbenzene spectrum analysis), hexamethylbenzene spectrum analysis: using GC-9800 gas chromatograph, the column specification is 30m×Φ0.32mm...

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Abstract

The invention relates to a method for preparing hexamethylbenzene by taking 2-butyne as a raw material in the technical field of organic synthesis. The method comprises the following step: in the presence of a palladium chloride catalyst and a copper chloride cocatalyst, taking 2-butyne and a solvent, carrying out reaction at normal pressure and at 45-65 DEG C to obtain hexamethylbenzene, wherein the mass ratio of the palladium chloride catalyst to 2-butyne is 1: (10-15), the mass ratio of the palladium chloride catalyst to the copper chloride cocatalyst is 1: (3-6), and the mass ratio of the solvent to 2-butyne is (3-8): 1. The production process provided by the invention is mild in reaction condition and only stirring at 45-65 DEG C is needed. The production process provided by the invention is relatively high in yield which is near 60%. Compared with the yield (20-30%) of the conventional process, the yield is nearly doubled. The production process and operation are relatively simple and convenient, the utilization ratio of raw materials is high, and less byproducts and three wastes (waste water, waste gas and industrial residue) are generated.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing hexamethylbenzene by using 2-butyne as a raw material. Background technique [0002] Aromatic rings are important structural units of many organic molecules, and polysubstituted benzene derivatives are an important class of aromatic ring compounds. Many substituted benzene derivatives are important components of molecules with physiological properties or medicinal properties or polymeric molecules, and are also important synthetic intermediates. Therefore, both in industrial production and laboratory work, aromatic ring compounds have a wide range of uses. As a new class of aromatic compounds, hexa-substituted benzene has received extensive attention. Hexamethylbenzene, colorless flaky crystal. The melting point is 166-167°C (165.5°C), the boiling point is 265°C, and the relative density is 1.0630 (25 / 4°C). It is easily soluble in e...

Claims

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Application Information

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IPC IPC(8): C07C15/02C07C2/48
Inventor 虞明东许泽陈超
Owner SHANGHAI CHENGYING NEW MATERIALS
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