Method for preparing diiodomethane by solid-supported phase transfer catalyst

A technology of phase transfer catalyst and diiodomethane, which is applied in the direction of halogen substitution preparation, chemical recovery, organic chemistry, etc., can solve the problems that phase transfer catalyst cannot be recovered, the reaction conditions are harsh, and solvent recovery is difficult, so as to improve catalyst performance and operation Simplicity and the effect of shortening the reaction time

Inactive Publication Date: 2012-01-18
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem solved by the present invention is to provide a method for preparing diiodomethane with a solid-supported phase transfer catalyst, so as to overcome the disadvantages in the prior art that the reaction conditions are harsh, the operation is cumbersome, the solvent recovery is difficult, and the phase transfer catalyst cannot be recovered.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 332g 50wt% potassium iodide solution, 38.6g dichloromethane and 10g immobilized phase transfer catalyst respectively in the reactor with heating, stirring and thermometer, heat up under stirring, and react at 72±2°C for 10 hours The reaction solution is cooled to 30°C, and the solid-supported phase transfer catalyst is removed by filtration (the catalyst can be recycled and reused); the organic layer is separated with a water separator, and 200ml of 5wt% sodium thiosulfate solution is added successively for washing, and 400ml of water is added for washing , adding anhydrous sodium sulfate for drying, the obtained oily product was distilled under reduced pressure, and the fractions under the condition of 89-92°C / 50mmHg were collected to obtain 99.83g of diiodomethane, with a yield of 82.0% and a content of 99.3% (HPLC).

Embodiment 2

[0018] Add 277g 60wt% potassium iodide solution, 35.4g dichloromethane and 8g immobilized phase transfer catalyst respectively in the reactor with heating, stirring and thermometer, heat up under stirring, and react at 90±2°C for 8 hours The reaction solution is cooled to 40°C, and the solid-supported phase transfer catalyst is removed by filtration (the catalyst can be recycled and reused); the organic layer is separated with a water separator, and 200ml of 5wt% sodium thiosulfate solution is added for washing successively, and 400ml of water is added for washing , adding anhydrous sodium sulfate for drying, the obtained oily product was distilled under reduced pressure, and the cuts under the condition of 89-92°C / 50mmHg were collected to obtain 94.42g of diiodomethane, with a yield of 84.6% and a content of 99.1% (HPLC).

Embodiment 3

[0020] Add 237g 70wt% potassium iodide solution, 32.7g methylene chloride and 6.8g immobilized phase transfer catalyst respectively in the reactor with heating, stirring and thermometer, heat up under stirring, and react at 108±2°C for 7 hour; the reaction solution is cooled to 50°C, and the immobilized phase transfer catalyst is removed by filtration (the catalyst can be recycled and reused); the organic layer is separated with a water separator, and 200ml 5wt% sodium thiosulfate solution is added successively for washing, and 400ml water is added for further washing. Wash with water, add anhydrous sodium sulfate to dry, the obtained oily product is distilled under reduced pressure, collect the distillate under the condition of 89-92 ℃ / 50mmHg, obtain diiodomethane 92.71g, the yield is 90.0%, the content is 99.5% (HPLC).

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Abstract

The invention discloses a method for preparing diiodomethane by a solid-supported phase transfer catalyst, in which potassium iodide and dichloromethane are used as raw materials, exchange reaction is carried out in the presence of the solid-supported phase transfer catalyst, and target products are collected from reacted organic phases. The content of the diiodomethane obtained in the preparing method disclosed by the invention reaches more than 99%, and the yield reaches more than 80%. Compared with the prior art, the performance of the catalyst is improved by the solid-supported phase transfer catalyst, and the reaction time is shortened; and the solid-supported phase transfer catalyst can be recycled and reused, the production cost is reduced, a product has stable quality and high purity, and the method is suitable for continuous production.

Description

technical field [0001] The invention relates to a method for preparing diiodomethane, in particular to a method for preparing diiodomethane with a solid-supported phase transfer catalyst. Background technique [0002] Diiodomethane is an important chemical basic product, widely used in organic synthesis, mineral analysis and separation, etc., especially for the reaction of synthesizing cyclopropane. [0003] In the prior art, the preparation method of diiodomethane adopts dichloromethane and sodium iodide to carry out substitution reaction in DMF solvent and obtains, but the reaction needs to be carried out under anhydrous conditions, and the operation is cumbersome, and using DMF as a solvent is not conducive to environmental protection, Difficulty in recovery; "Chemical Reagent" 1983 (5): in 41, Sun Chang'an etc. adopt phase-transfer catalysis method, take benzyl triethyl ammonium chloride as phase-transfer catalyst, dichloromethane and sodium iodide and phase-transfer cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/07C07C17/20
CPCY02P20/584
Inventor 王伟顾小焱吕明王永旗
Owner TAICANG HUSHI REAGENT
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