ChemicalBook CAS DataBase List Perfluoro(4-methyl-3,6-dioxaoct-7-ene)sulfonyl fluoride

Perfluoro(4-methyl-3,6-dioxaoct-7-ene)sulfonyl fluoride synthesis

4synthesis methods

Product Name:Perfluoro(4-methyl-3,6-dioxaoct-7-ene)sulfonyl fluoride
CAS Number:16090-14-5
Molecular formula:C7F14O4S
Molecular Weight:446.12

(1) Intermediate synthesis In a 1L reactor, add 100ml of dimethylacetamide, 8g of potassium fluoride, and 200g (1.11mol) of tetrafluoroethane-β-sultone,Subsequently, 500g (3mol) of hexafluoropropylene oxide was introduced at a flow rate of 0.3kg/h for addition reaction, and the reaction temperature was controlled at 20°C.The reaction pressure is controlled at 0.4MPa. After the introduction of hexafluoropropylene oxide is completed, the reaction is continued for 1 hour. After the reaction is completed,The reaction liquid was rectified to obtain 528g (1.03mol) of intermediate, with a yield of 92% and a purity of 99.1%;(2) PSVE synthesis In a moving bed reactor (volume 2L, material 316L, produced by Tianjin Qixi Technology Co., Ltd.),A mixture of 500g (0.97mol) of the intermediate obtained in step (1) and 600g of potassium carbonate (4.34mol) was passed through the salt formation zone and decarboxylation zone of the moving bed reactor in turn (the salt formation temperature was set to 150°C,The decarboxylation temperature is set to 360°C) to carry out the salt formation reaction and the decarboxylation reaction, and the contact time of the salt formation reaction is 10 min by controlling the material feed rate.The contact time of the decarboxylation reaction is 25min, and the decarboxylation reaction product is collected by condensation to obtain a crude product.The crude product is rectified to obtain the product perfluoro-3,6-dioxa-4-methyl-7-octenesulfonyl fluoride with a purity of 98.5% and a yield of 85%.

428-59-1 Synthesis

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Perfluoro(4-methyl-3,6-dioxaoct-7-ene)sulfonyl fluoride

16090-14-5
109 suppliers
$55.00/1g

Yield:16090-14-5 85%

Reaction Conditions:

Stage #1: Hexafluoropropene oxide;tetrafluoroethane-β-sultonewith potassium fluoride in N,N-dimethyl acetamide at 20; under 3000.3 Torr; for 1 h;
Stage #2: with potassium carbonate at 150 - 360; for 0.583333 h;Pressure;Temperature;Solvent;Reagent/catalyst;

Steps:

1.1-1.2; 2.1-2.2; 3.1; 3.2; 4.1-4.2

(1) Intermediate synthesis In a 1L reactor, add 100ml of dimethylacetamide, 8g of potassium fluoride, and 200g (1.11mol) of tetrafluoroethane-β-sultone,Subsequently, 500g (3mol) of hexafluoropropylene oxide was introduced at a flow rate of 0.3kg/h for addition reaction, and the reaction temperature was controlled at 20°C.The reaction pressure is controlled at 0.4MPa. After the introduction of hexafluoropropylene oxide is completed, the reaction is continued for 1 hour. After the reaction is completed,The reaction liquid was rectified to obtain 528g (1.03mol) of intermediate, with a yield of 92% and a purity of 99.1%;(2) PSVE synthesis In a moving bed reactor (volume 2L, material 316L, produced by Tianjin Qixi Technology Co., Ltd.),A mixture of 500g (0.97mol) of the intermediate obtained in step (1) and 600g of potassium carbonate (4.34mol) was passed through the salt formation zone and decarboxylation zone of the moving bed reactor in turn (the salt formation temperature was set to 150°C,The decarboxylation temperature is set to 360°C) to carry out the salt formation reaction and the decarboxylation reaction, and the contact time of the salt formation reaction is 10 min by controlling the material feed rate.The contact time of the decarboxylation reaction is 25min, and the decarboxylation reaction product is collected by condensation to obtain a crude product.The crude product is rectified to obtain the product perfluoro-3,6-dioxa-4-methyl-7-octenesulfonyl fluoride with a purity of 98.5% and a yield of 85%.

References:

CN112250603,2021,A Location in patent:Paragraph 0031-0050