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Synthetic method of difluoroacetyl fluoride

A technology of difluoroacetyl fluoride and synthesis method, which is applied in the field of synthesis of difluoroacetyl fluoride, can solve the problems of harsh fluorination reaction conditions, difficult operation, and high cost, and achieve the advantages of simple operation, lower reaction temperature, and simplified production process Effect

Pending Publication Date: 2020-11-27
SUQIAN KEYLAB BIOCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above two methods are relatively harsh for the preparation of raw materials and the final fluorination reaction conditions, and often need to be reacted in a high temperature environment above 200 ° C, which is difficult to operate and high in cost.

Method used

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  • Synthetic method of difluoroacetyl fluoride
  • Synthetic method of difluoroacetyl fluoride
  • Synthetic method of difluoroacetyl fluoride

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preparation example Construction

[0034] The preparation method of chromium complex catalyst among the present invention can refer to following documents and books:

[0035] (1) Efficient, Single-Step Access to Imidazo[1,5-a]pyridine N-Heterocyclic Carbene Precursors[J].ORGANIC LETTERS.2011Vol.13,No.19 5256–5259;

[0036] (2)(C ∧ C * )-cyclometalated platinum(II)imidazo[1,5-a]pyridine NHC complexes-Synthesis and characterization[J].Journal of Organometallic Chemistry.775(2015).155-163;

[0037] (3) Efficient synthesis of bulky N-Heterocyclic carbene ligands forcoinage metal complexes[J].Journal of Organometallic Chemistry.820(2016).1-7;

[0038] (4)Synthesis and characterization of novel cyclopentadienylmolybdenum imidazo[1,5-a]pyridine-3-ylidene complexes and their applicationin olefin oxidation catalysis[J].Journal of Catalysis.319(2014).119–126;

[0039] (5) Chiral imidazo[1,5-a]tetrahydroquinoline N-heterocyclic carbenes and their copper complexes for asymmetric catalysis[J].Tetrahedron:Asymmetry.24(201...

Embodiment 1

[0042]The concrete steps of the synthetic method of the difluoroacetyl fluoride of present embodiment are:

[0043] Step 1. Add 1314g (10mol) of trichlorethylene and 19.6g (0.2mol) of triethylboron in the pressure reactor, then feed dry oxygen, and adjust the pressure of oxygen to 3 atmospheres, then heat up Reaction at 80°C for 10h. After the reaction was completed, atmospheric distillation was carried out, and fractions were collected at a temperature range of 105° C. to 108° C. to obtain 1316 g of a colorless and transparent liquid product, dichloroacetyl chloride, with a yield of 89%. The product was analyzed by gas chromatography and was consistent with the standard sample. The reaction formula is as follows:

[0044]

[0045] Step 2. Add 147g (1mol) of dichloroacetyl chloride, 130g of sodium fluoride and 7.4g (0.01mol) of chromium complex catalyst into the pressure reactor, connect the valve and gas conduit, and heat up to 80°C. Open the valve after reacting for 2 ...

Embodiment 2

[0059] The concrete steps of the synthetic method of the difluoroacetyl fluoride of present embodiment are:

[0060] Step 1. Add 1314g (10mol) of trichlorethylene and 18.2g (0.1mol) of tributylboron into the pressure-resistant reactor, then feed dry oxygen, and adjust the pressure of oxygen to 3 atmospheres, then raise the temperature Reaction at 80°C for 11h. After the reaction was completed, atmospheric distillation was carried out, and fractions were collected at a temperature range of 105° C. to 108° C. to obtain 1325 g of a colorless and transparent liquid product, dichloroacetyl chloride, with a yield of 90%. The product was analyzed by gas chromatography and was consistent with the standard sample. The reaction formula is as follows:

[0061]

[0062] Step 2: Add 147g (1mol) of dichloroacetyl chloride, 180g of potassium fluoride and 6.9g (0.01mol) of chromium complex catalyst into the pressure-resistant reactor, connect the valve and gas conduit, and heat up to 80°...

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Abstract

The invention relates to a synthesis method of difluoroacetyl fluoride, which comprises the following steps: 1. reacting trichloroethylene with oxygen under the catalytic action of trialkyl boron shown in the formula I to generate dichloroacetyl chloride, and 2. reacting dichloroacetyl chloride with inorganic fluoride shown in the formula II under the action of a catalyst to generate difluoroacetyl fluoride. According to the synthetic method of difluoroacetyl fluoride, the raw materials are simple and easy to obtain, high-temperature reaction is not needed, and the yield is high.

Description

technical field [0001] The invention relates to a synthesis method of difluoroacetyl fluoride, which belongs to the technical field of chemical synthesis. Background technique [0002] Difluoroacetyl fluoride (CAS No. 2925-22-6) is an important intermediate in organic synthesis, which is widely used in the synthesis of medicine, pesticides, and fine chemicals. For the synthesis method of difluoroacetyl fluoride, there are mainly two types of methods at present: (1) Japanese patent document JP2011168564, Korean patent document KR1789771 and European patent document EP0694523 etc. have reported the method of utilizing tetrafluoroethyl ether to prepare difluoroacetyl fluoride; (2) WO2009115426 reports a method for preparing difluoroacetyl fluoride from dichloroacetyl chloride, the reaction formula of which is as follows: [0003] [0004] The above two methods are relatively harsh for the preparation of raw materials and the final fluorination reaction conditions, and often...

Claims

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Application Information

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IPC IPC(8): C07C53/48C07C51/363B01J31/22
CPCC07C51/363C07C51/25B01J31/2273B01J2531/0241B01J2531/62C07C53/48Y02P20/584
Inventor 王明春李庆毅林韦康陈东辉
Owner SUQIAN KEYLAB BIOCHEMICAL CO LTD
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