Method of synthesizing fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether

A technology for the synthesis of hexafluoroisopropyl ether, which is applied in chemical instruments and methods, preparation of ether, preparation of organic compounds, etc., can solve the problems of high price and danger, and achieve low price, easy removal, handling and operation easy effect

Inactive Publication Date: 2007-10-24
SHANGHAI HUMEI CHEM IND TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the synthetic methods of these two U.S. patents US6469219 and US5705710, all use the strong active oxidation fluorinating agent bromine trifluoride Br 3 F, this reagent is expensive and has certain risks

Method used

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  • Method of synthesizing fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether

Examples

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Embodiment 1

[0026]A 50L glass reactor with a lower outlet was used, with a set of mechanical stirring devices, a thermocouple, an internal coil and a refrigeration compressor. Add 3556g (25.86mol) of phosphorus trichloride, lower the system to 0°C and add 4345g (48.28mol) of HFIP while stirring, continue stirring until the HCl gas is exhausted, then add 1,3,5-trioxane 2327g (25.86mol). The temperature will rise to about 8°C, but then it will drop back to 0°C, and the stirring reaction will continue for 8 hours. Then began to slowly add 4L of 6N HCl dropwise. The reaction is an exothermic reaction, so the temperature will rise and be maintained at 45°C. Then add 5L of deionized water and stir until all the solids are dissolved and the system is clearly divided into two layers. The bottom layer is taken out to obtain the product chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether.

Embodiment 2

[0028] A 50L glass reactor was used with a mechanical stirring device, a thermocouple and a thermostatic jacket. Dissolve 7031g (32.48mol) of chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether in 16L dimethyl sulfoxide and continue stirring, while stirring, add 1364g (32.48mol) of NaF It was fluorinated, then heated to 30°C and reacted for 1h. Add 5 L of deionized water and stir until the solution is clearly divided into two layers, then take out the bottom layer to obtain the product sevoflurane.

Embodiment 3

[0030] A dry 250ml round bottom flask was used with a PTFE stir bar, a thermometer and a freezer. Open the freezer to freeze, make the system temperature drop to 0 ℃, add aluminum trichloride 18.6g (0139mol), HFIP31.2g (0.186mol) in the flask, pass N 2 Bubble for ten minutes to drive away the HCl gas that is not conducive to the reaction in the system. Then add 4.18 g (0.034 mol) of paraformaldehyde, turn off the freezer, let it rise to room temperature freely and start stirring. After reacting for 12 hours, add 50ml of 6N HCl dropwise. After the dropwise addition, add 50ml of deionized water and pour it into a separatory funnel for layering. After taking out the bottom clear liquid, the product chloromethyl-1,1,1 , 3,3,3-Hexafluoroisopropyl ether.

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Abstract

The invention discloses a synthesizing method of fluomethyl-1,1,1,3,3,3-hexafluoroisopropyl ether, which comprises the following steps: 1) reacting 1,1,1,3,3,3-hexafluorine-2-propanol and ,3,5-trioxymethylene or oligoformaldehyde and Lewis acid chloride to generate chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether as intermediate and HOAlCl2 as by-product; adding 6N HCl to disintegrate to remove by-product HOAlCl2; 2) reacting chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether and fluorination agent and solvent to produce the product; improving the selectivity of intermediate; removing by-product easily.

Description

technical field [0001] The invention relates to a synthesis method of fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether. Background technique [0002] Fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether, molecular formula (CF 3 ) 2 CHOCH 2 F, referred to as sevoflurane. [0003] In recent years, it has been found that fluorinated ethers are well suited for use in the field of inhalational anesthetics. These substances roughly have desflurane (CF 3 CHFOCH 2 F), isoflurane (CF 3 CHClOCHF 2 ), isoflurane (HClFCCF 2 OCHF 2 ) and fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether ((CF 3 ) 2 CHOCH 2 F) These types. Among them, fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether (hereinafter referred to as sevoflurane) has the characteristics of inducing anesthesia and waking up quickly, and can also reduce cerebrovascular resistance, brain metabolic rate, Cerebral oxygen consumption, myocardial contractility and blood pressure are significantly less irritating to the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C41/22C07C43/04
Inventor 方人杰刘红阳
Owner SHANGHAI HUMEI CHEM IND TECH DEV
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