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Preparation method of diiodomethane

A technology of diiodomethane and dichloromethane, which is applied in the field of preparation of halogenated fine chemicals, can solve the problems of high production cost, large amount of high-concentration salt-containing waste water, unreusable catalysts, etc. The effect of production costs

Inactive Publication Date: 2021-06-15
浙江肯特催化材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the deficiencies of the prior art, and to provide a method for preparing diiodomethane by solid-liquid phase transfer catalysis. The problem of large amount and high production cost is a kind of preparation method of diiodomethane

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  • Preparation method of diiodomethane

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Effect test

Embodiment 1

[0024] Example 1: 250 g of dichloromethane, 3.9 g of triethylbenzyl ammonium chloride and 300 g of distilled water were successively added into a reactor with stirring, 1080 g of sodium iodide was added in batches under stirring, and the temperature was raised to 105-110°C , maintain the reaction for 12 hours, after gas chromatographic analysis of the sample, cool down to about 50°C, and suction filter the precipitated sodium chloride solid. The filtrate was left to stand for stratification, and the lower organic layer was separated, and the upper aqueous layer was reserved for the next application. The organic layer was washed with 250ml of 5% sodium thiosulfate solution, washed once with 200ml of water, and dried over anhydrous sodium sulfate. The obtained light yellow oil was subjected to vacuum fractionation, the vacuum degree was controlled at 20-30 mm Hg, and the bath temperature was not more than 90° C. to obtain 585.1 g of diiodomethane product with a yield of 74.2% an...

Embodiment 2

[0025] Embodiment 2: above-mentioned water layer (containing unreacted sodium iodide 63.0g and triethylbenzyl ammonium chloride 3.9g) directly drops into next batch reaction, adds dichloromethane 250g, adds sodium iodide 1017g, heats up Keep the reaction at 105-110°C for 12 hours. After sample gas chromatographic analysis, cool down to about 50°C, and suction filter the precipitated sodium chloride solid. The filtrate was left to stand for stratification, and the lower organic layer was separated, and the upper aqueous layer was reserved for the next application. The organic layer was washed with 250ml of 5% sodium thiosulfate solution, washed once with 200ml of water, and dried over anhydrous sodium sulfate. The light yellow oil was subjected to fractional distillation under reduced pressure to obtain 564.5 g of diiodomethane product with a yield of 71.7% and a purity of 99.1% (GC).

Embodiment 3

[0026] Example 3: Add 250 g of dichloromethane, 3.9 g of triethylbenzyl ammonium chloride and 200 g of distilled water successively into a reactor with stirring, add 1080 g of sodium iodide in batches under stirring, and heat up to 105-110°C , maintain the reaction for 12 hours, after gas chromatographic analysis of the sample, cool down to about 50°C, and suction filter the precipitated sodium chloride solid. The filtrate was left to stand for stratification, and the lower organic layer was separated, and the upper aqueous layer was reserved for the next application. The organic layer was washed with 250ml of 5% sodium thiosulfate solution, washed once with 200ml of water, and dried over anhydrous sodium sulfate. The obtained light yellow oil was fractionated under reduced pressure, the vacuum degree was controlled at 20-30 mm Hg, and the bath temperature was not more than 90° C. to obtain 602.5 g of diiodomethane product with a yield of 76.5% and a purity of 99.5% (GC).

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Abstract

The invention discloses a method for preparing diiodomethane through a solid-liquid phase transfer catalytic reaction. The method is characterized in that sodium iodide and dichloromethane are used as raw materials, and a solid-liquid phase transfer catalysis reaction is improved on the basis of liquid-liquid phase transfer catalysis, so that the recycling of a catalyst and sodium iodide is realized. Compared with the prior art, the method greatly reduces production cost and wastewater discharge, and realizes clean production.

Description

technical field [0001] The invention relates to a preparation method of halogenated fine chemicals, in particular to a preparation technology of diiodomethane. Background technique [0002] Diiodomethane is a widely used fine chemical, used in the determination of mineral density and refractive index, mineral separation and other fields. It is also widely used in pharmaceutical and chemical engineering, and is often used in the Simmons-Smith reaction for the synthesis of cyclopropane derivatives. For example, in the synthesis process of saxagliptin for the treatment of adult type 2 diabetes, it is used to construct cyclopropane rings stereoselectively. [0003] The existing diiodomethane preparation technology is usually obtained by the halogen exchange reaction between dichloromethane and sodium iodide in an organic solvent. The solvents used include benzyl alcohol, acetone, dimethylformamide, etc., and the reaction needs to be carried out under anhydrous conditions. Carry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C19/07
CPCC07C17/208C07C19/07Y02P20/584
Inventor 卓广澜王高郑琪杨建锋
Owner 浙江肯特催化材料科技有限公司
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