Imidodisulfurylfluoride synthesis

15873-42-4 Synthesis

15873-42-4
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7664-39-3 Synthesis

7664-39-3
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14984-73-7
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Yield: 89%

Reaction Conditions:

with chlorosulfonic acid;isocyanate de chlorosulfonyle at 160; under 60006 Torr; for 0.25 h;Reagent/catalyst;Temperature;Pressure;Time;

Steps:

1
The examples were carried out with DEVICE 1-0-HF: piston pump 260D from ISCO Teledyne DEVICE 1-0-MIXTRIP: piston pump 260D from ISCO Teledyne DEVICEl-1 being a 1/8 inch coiled tube with internal volume VOLUME 1 of 3.8 ml made of hastelloy C. For the heating a coiled-tube-in-container set up was used. Heating medium was conventional oil. DEVICEl-2 being a 1/8 inch tube with ca. 1.5 mL internal volume made of hastelloy C. Cooling was done by simply contact of the tube with the air having room temperature. • DEVICEl-3: pneumatically controlled valve from SAMSON Microvalve type 3510-7 with a Cv value of 0.01. • DEVICE 1-4: any gaseous components, which are essentially HC1 and excess HF, were separated from the reaction mixture in a vented vessel made of stainless steel. MIXTURE-TRIPLE-90-5-5 was fed simultaneously with HF into DEVICEl-1 at a PRESSUREl-1 of 80 bar, MIXTURE-TRIPLE-90-5-5 was fed by DEVICE 1-0-MIXTRIP at a flow rate of 0.118 ml/min, and HF was fed by DEVICE 1-0-HF with at a flow rate of 0.137 ml/min. TIME 1-1 was approximately 15 min, TEMPl-1 was 160°C. The molar ratio of HF : MIXTURE-TRIPLE-90-5-5 resulting from the flow rates was approximately 8 : 1. Then the reaction mixture from DEVICEl-1 was cooled to TEMP 1-2 in DEVICE 1-2, TEMP 1-2 was room temperature, TIME 1-2 was approximately 5.9 min, and was then expanded by DEVICEl-3 into DEVICEl-4. The liquid collected was HFSI confirmed by ¹⁹F NMR. The yield was 89% based on compound of formula (2) in MIXTURE-TRIPLE-90-5-5.

References:

LONZA LTD;SCHNIDER, Christian;HORMES, Anna-Christina;KLEIN, Andreas;BERSIER, Michael;STUDER, Philipp;TILLE, Stefan;GRUETZNER, Thomas WO2016/177765, 2016, A1 Location in patent:Page/Page column 26; 27

999-97-3 Synthesis