Synthesizing method of fluorine-containing iodoalkane

A synthesis method and technology of iodoalkane, which is applied in the field of synthesis of fluorine-containing iodoalkane, can solve problems such as low yield, and achieve the effects of high product purity, good reaction selectivity, and good operation safety

Inactive Publication Date: 2011-10-19
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Disclosed in CN 1182092 is a kind of trifluorochloroethane and sodium iodide or potassium iodide as main raw materials, under the existence of quaternary ammonium salt or polyethylene glycol phase transfer catalyst and in the aprotic polar solvent, synthesized trifluoroiodide Ethane, but in low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 4 g 18-crown-6, 3 mol CF to a 1.0 L reactor 2 HCH 2 CH 2 CH 2 After adding Cl and 1 mol of sodium iodide, seal the reaction vessel. Stirring was started, the temperature of the reactor was raised to 85°C, and the reaction was carried out at constant temperature for 5 h. The reactant was filtered and rectified to obtain CF 3 CH 2 CH 2 CH 2 1, the yield based on sodium iodide is 94.3%.

Embodiment 2

[0023] Add 5.5 mol CF to a 1.0 L reactor 3 CH 2 CH 2 CH 2 CH 2 After adding Br, 2 mol of sodium iodide and 500ml of acetone, seal the reaction kettle. Stirring was started, the temperature of the reactor was raised to 70°C, and the reaction was carried out at constant temperature for 6 h. The reactant was filtered and rectified to obtain CF 3 CH 2 CH 2 CH 2 CH 2 1, the yield based on sodium iodide is 80.5%.

Embodiment 3

[0025] Add 1.5 g tetramethylammonium bromide, 3 mol CF 2HCH 2 CH 2 Cl, 3mol sodium iodide and 500 ml butanone, seal the reaction kettle. Stirring was started, the temperature of the reactor was raised to 75°C, and the reaction was stopped after constant temperature reaction for 6 h. The reactant was filtered and rectified to obtain CF 2 HCH 2 CH 2 1, the yield based on sodium iodide is 88.9%.

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Abstract

The invention discloses a synthesizing method of fluorine-containing iodoalkane. The synthesis is carried out under the effect of a phase-transfer catalyst, and/or in a polar aprotic ketone solvent. A compound with a general formula of CFmH3-m(CH2)nX is subject to a halogen exchange reaction with sodium iodide or potassium iodide, such that a compound with a general formula of CFmH3-m(CH2)nI is synthesized, wherein m=2 to 3, n=2 to 5, and X represents Cl or Br. The reaction temperature is 20 DEG C to 140 DEG C. The mass ratio of the phase-transfer catalyst to CFmH3-m(CH2)nX is 0.0005:1 to 0.05:1. The molar ratio of CFmH3-m(CH2)nX to sodium iodide or potassium iodide is 0.5:1 to 5:1. The method provided by the present invention has substantial advantages of short process procedures, and low raw material cost.

Description

technical field [0001] The invention relates to the technical field of synthesis, in particular to a method for synthesizing fluorine-containing iodoalkanes. Background technique [0002] The C-I bond in fluorinated iodoalkanes is relatively active, making it easier to synthesize other chemicals. Therefore, it has become an important fluorine-containing building block reagent, and is mainly used as an intermediate in medicine and medicine synthesis. [0003] Disclosed in CN 1182092 is a kind of trifluorochloroethane and sodium iodide or potassium iodide as main raw materials, under the existence of quaternary ammonium salt or polyethylene glycol phase transfer catalyst and in the aprotic polar solvent, synthesized trifluoroiodide ethane, but in lower yields. [0004] In this method, a phase transfer catalyst and an aprotic solvent are necessary conditions for the fluorine-chlorine exchange reaction, and the solvents used are N,N-dimethylformamide, dimethyl sulfoxide and N-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/16C07C17/20
Inventor 周强吴庆王树华
Owner JUHUA GRP
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