Described herein are methods and devices that allow the generation of [F-18]triflyl fluoride and other [F-18] sulfonyl fluorides (such as [F-18]tosyl fluoride) in a manner that is suitable for radiosynthesis of F-18 labeled radiopharmaceuticals using currently available synthesis modules.

Described herein are methods and devices that allow the generation of [F-18]triflyl fluoride and other [F-18] sulfonyl fluorides (such as [F-18]tosyl fluoride) in a manner that is suitable for radiosynthesis of F-18 labeled radiopharmaceuticals using currently available synthesis modules.

The invention relates to a process for working up water containing 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone as impurities, comprising: (a) mixing the water containing 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone as impurities with an organic solvent in which 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone have a solubility of at least 0.5 wt % based on the amount of 4,4′-dichlorodiphenyl sulfoxide and/or 4, 4′-dichlorodiphenyl sulfone and organic solvent at 20° C., which forms a two-phase system with water and which can be stripped from water with a stripping gas and subsequently separating the obtained mixture into an aqueous phase and an organic phase, and (b) stripping the organic solvent from the aqueous phase with a stripping gas.

The invention relates to a process for working up water containing 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone as impurities, comprising: (a) mixing the water containing 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone as impurities with an organic solvent in which 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone have a solubility of at least 0.5 wt % based on the amount of 4,4′-dichlorodiphenyl sulfoxide and/or 4, 4′-dichlorodiphenyl sulfone and organic solvent at 20° C., which forms a two-phase system with water and which can be stripped from water with a stripping gas and subsequently separating the obtained mixture into an aqueous phase and an organic phase, and (b) stripping the organic solvent from the aqueous phase with a stripping gas.

Disclosed is a method for preparing β-carbonyl sulfones. The method comprises: by taking an α-carbonyl diazo compound and sodium arylsulfinate as reaction substrates, cheap silver nitrate as an optimal catalyst, 1,10-phenanthroline as a ligand, and potassium persulfate as an oxidant, carrying out coupling reaction in a mixed solvent of acetonitrile and water to obtain a β-carbonyl sulfones compound. Compared with the prior art, the method has the following advantages: a wide range of reaction substrates, short reaction time, a relatively high reaction yield, a mild reaction condition, etc. In the present invention, non-toxic and harmless reagents are used as reaction raw materials, so that it has no harm to the environment and satisfies the requirements of contemporary green chemistry development. Post-reaction treatment is relatively simple, and is convenient for separation and purification. In addition, the reaction can achieve gram-scale synthesis, and lays a foundation for actual applications.

Disclosed is a method for preparing β-carbonyl sulfones. The method comprises: by taking an α-carbonyl diazo compound and sodium arylsulfinate as reaction substrates, cheap silver nitrate as an optimal catalyst, 1,10-phenanthroline as a ligand, and potassium persulfate as an oxidant, carrying out coupling reaction in a mixed solvent of acetonitrile and water to obtain a β-carbonyl sulfones compound. Compared with the prior art, the method has the following advantages: a wide range of reaction substrates, short reaction time, a relatively high reaction yield, a mild reaction condition, etc. In the present invention, non-toxic and harmless reagents are used as reaction raw materials, so that it has no harm to the environment and satisfies the requirements of contemporary green chemistry development. Post-reaction treatment is relatively simple, and is convenient for separation and purification. In addition, the reaction can achieve gram-scale synthesis, and lays a foundation for actual applications.

The invention relates to a process for purifying crude 4,4′-dichlorodiphenyl sulfone comprising: (a) dissolving the crude 4,4′-dichlorodiphenyl sulfone which may contain water in an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C. and optionally adding water to obtain a solution which comprises 4,4′-dichlorodiphenyl sulfone, the organic solvent and 1 to 30 wt % water based on the amount of 4,4′-dichlorodiphenyl sulfone and water; (b) cooling the solution to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfone to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone; (c) carrying out a solid-liquid separation to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfone and a mother liquor; (d) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C.; (e) optionally repeating steps (b) to (d); (f) drying the 4,4′-dichlorodiphenyl sulfone.

The invention relates to a process for purifying crude 4,4′-dichlorodiphenyl sulfone comprising: (a) dissolving the crude 4,4′-dichlorodiphenyl sulfone which may contain water in an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C. and optionally adding water to obtain a solution which comprises 4,4′-dichlorodiphenyl sulfone, the organic solvent and 1 to 30 wt % water based on the amount of 4,4′-dichlorodiphenyl sulfone and water; (b) cooling the solution to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfone to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone; (c) carrying out a solid-liquid separation to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfone and a mother liquor; (d) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C.; (e) optionally repeating steps (b) to (d); (f) drying the 4,4′-dichlorodiphenyl sulfone.

The invention relates to a process for purifying crude 4,4′-dichlorodiphenyl sulfone comprising: (a) dissolving the crude 4,4′-dichlorodiphenyl sulfone which may contain water in an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C. and optionally adding water to obtain a solution which comprises 4,4′-dichlorodiphenyl sulfone, the organic solvent and 1 to 30 wt % water based on the amount of 4,4′-dichlorodiphenyl sulfone and water; (b) cooling the solution to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfone to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone; (c) carrying out a solid-liquid separation to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfone and a mother liquor; (d) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C.; (e) optionally repeating steps (b) to (d); (f) drying the 4,4′-dichlorodiphenyl sulfone.

The invention relates to a process for purifying 4,4′-dichlorodiphenyl sulfone comprising: (a) providing a suspension comprising particulate 4,4′-dichlorodiphenyl sulfone in carboxylic acid, (b) carrying out a solid-liquid separation of the suspension to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfone and a carboxylic acid comprising filtrate, (c) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an aqueous base and then with water, (d) mixing the aqueous base after being used for washing with a strong acid, or mixing the aqueous base after being used for washing, the carboxylic acid comprising filtrate and a strong acid, (e) carrying out a phase separation in which an aqueous phase and an organic phase comprising the carboxylic acid are obtained.