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Method for fluoridating diethylaminosulphur trifluoride at low temperature

A technology for fluorinating diethylaminosulfur trifluoride and diethylaminosulfur trifluoride, which is applied in the field of low-temperature diethylaminosulfur trifluoride fluorination, can solve problems such as limited application fields, and achieve reliable reaction Strong controllability, convenient preparation and simple process

Inactive Publication Date: 2012-07-11
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Low-temperature diethylaminosulfur trifluoride fluoride plays an important role, which can make the reaction more moderate and controllable, and prevent the explosion hazard in the preparation process, but its application field is still limited

Method used

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  • Method for fluoridating diethylaminosulphur trifluoride at low temperature
  • Method for fluoridating diethylaminosulphur trifluoride at low temperature
  • Method for fluoridating diethylaminosulphur trifluoride at low temperature

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Embodiment 1

[0024] A method for low-temperature fluorination of diethylaminosulfur trifluoride, comprising the following steps:

[0025] Put it in a polytetrafluoroethylene container, add 4-carboxypiperidine and diethylaminosulfur trifluoride (DAST, CAS: 38078-09-0) to fluoride at a low temperature of -6°C to form 4-trifluoroform Piperidine, the molar ratio of 4-carboxypiperidine to diethylaminosulfur trifluoride is 1:1.5, then stir at room temperature at 18°C, track the plate, and pour the lye NaHCO 3 in solution;

[0026]

[0027] Formula 2

[0028] The above reaction mixture was concentrated by distillation, and then precipitated with a solvent, filtered, washed and dried to obtain a reactant. For further processing, the reaction mixture can be filtered to remove the catalyst, and the obtained filtrate can be concentrated by distillation to remove ethanol. The temperature of the distillation concentration is 100° C., and the distillation can be carried out using a rotary evaporato...

Embodiment 2

[0032] A method for low-temperature fluorination of diethylaminosulfur trifluoride, comprising the following steps:

[0033] Put it in a polytetrafluoroethylene container, add 4-carboxypiperidine and diethylaminosulfur trifluoride (DAST, CAS: 38078-09-0) to fluoride at a low temperature of -1°C to form 4-trifluoroform Basepiperidine, the molar ratio of 4-carboxypiperidine to diethylaminosulfur trifluoride is 1:1.5, and ethanol is also included, and the molar ratio of ethanol in the 4-carboxypiperidine is 1:0.001. Then stir at room temperature 20°C, track on the spot plate, and pour NaHCO 3 In the solution; filter the above reaction mixture to remove the catalyst, and the obtained filtrate is concentrated by distillation to remove ether. The temperature of the distillation concentration is 200 ° C. The distillation and concentration steps can be carried out using a rotary evaporator, and the concentrate is an oily substance. Then washed with ether, dried in a drying oven at 15...

Embodiment 3

[0035] A method for low-temperature fluorination of diethylaminosulfur trifluoride, comprising the following steps:

[0036] (1) Preparation of 4-trifluoromethylpiperidine:

[0037] Put it in a polytetrafluoroethylene container, add 4-carboxypiperidine and diethylaminosulfur trifluoride (DAST, CAS: 38078-09-0) to fluoride at a low temperature of 0°C to form 4-trifluoromethyl For piperidine, the molar ratio of 4-carboxypiperidine to diethylaminosulfur trifluoride is 1:2, and ethanol is also included, and the molar ratio of the 4-carboxypiperidine to ethanol is 1:0.01. Then stir at room temperature 25°C, track on the spot plate, and pour the lye NaHCO after completion 3 In the solution; filter the reaction mixture in the above steps to remove the catalyst, and the obtained filtrate is concentrated by distillation to remove propylene glycol. The temperature of the distillation concentration is 150°C. Distillation. The distillation concentration step can use a rotary evaporator, ...

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Abstract

The invention discloses a method for fluoridating diethylaminosulphur trifluoride at a low temperature. The method comprises the following steps of: carrying out fluoridation on 4-carboxyl piperidine and the diethylaminosulphur trifluoride (DAST, CAS:38078-09-0) at the low temperature to produce 4-(trifluoromethyl)piperidine, wherein the molar ratio of the 4-carboxyl piperidine to the diethylaminosulphur trifluoride is 1:(1.5-2); stirring the 4-(trifluoromethyl)piperidine at room temperature, carrying out point-board tracking, and pouring the 4-(trifluoromethyl)piperidine into a lye solution after finishing the point-board tracking; and carrying out distillation and concentration on a reaction mixture obtained in the above steps, carrying out precipitation by using a solvent, and filtering, washing and drying to obtain reactants. The method has the advantages of simple process, strong reaction controllability, and convenience in preparation.

Description

technical field [0001] The invention relates to a method for low-temperature fluorination of diethylaminosulfur trifluoride, which belongs to the technical field of chemical industry. Background technique [0002] With the progress and development of the economy, the chemical industry has developed rapidly, providing many raw materials and intermediates for industry, agriculture and pharmaceutical industries, and widely used in the fields of medicine, dyes, oils, spices, and synthetic fibers. [0003] Low-temperature diethylaminosulfur trifluoride fluoride plays an important role, which can make the reaction more moderate and controllable, and prevent the danger of explosion during the preparation process, but its application field is still limited. Contents of the invention [0004] In order to solve the above problems, the present invention provides a method for low-temperature fluorination of diethylaminosulfur trifluoride, which is applied to the preparation of 4-trifl...

Claims

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Application Information

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IPC IPC(8): C07D211/20
Inventor 张巍朱虹
Owner SHANGHAI SINOFLUORO SCI
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