# US 10,246,409 B2 · Method for preparation of bis(fluorosulfonyl)-imide > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,246,409 B2 - Document ID: US10246409B2 - Status: Granted - Kind: B2 - Application number: 15/571,524 - Filed: 2016-05-04 - Published: 2018-05-24 - Granted: 2019-04-02 - Earliest claimed: 2015-05-06 - Assignees: Lonza Ltd. - Applicants: Lonza Ltd - Inventors: Christian Schnider; Anna-Christina Hormes; Andreas Klein; Michael Bersier; Philipp Studer; Stefan Tille; Thomas Gruetzner - Web page: https://patentgrep.com/patent/US10246409B2 ## CPC - C07C 303/40: by reactions not involving the formation of sulfonamide groups - B01J 19/0013: {Controlling the temperature of the process} - C01B 21/086: containing one or more sulfur atoms - C07C 303/36: of amides of sulfonic acids - C07C 311/48: having nitrogen atoms of sulfonamide groups further bound to another hetero atom - B01J 2219/00029: Batch processes - B01J 2219/00051: Controlling the temperature - B01J 2219/00162: controlling the pressure - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} ## Abstract The invention relates to a method for the preparation of bis(fluorosulfonyl)-imide and its derivatives at elevated temperature. ## Claims ### Claim 1 A method for the preparation of a compound of formula (I); the method comprises a step STEP1; STEP1 comprises a reaction REAC1-1; in REAC1-1 a mixture MIXTURE-TRIPLE is reacted with HF at a temperature TEMP1-1, TEMP1-1 is at least 80° C.; MIXTURE-TRIPLE comprises three components, a compound of formula (II), a compound of formula (III) and a compound of formula (IV); X is identical with X1 or with X2; X1 and X2 are identical or different and independently from each other selected from the group consisting of F, Cl, Br, I, RESF, and tolyl; wherein RESF is a fluorinated C1-9 alkyl, which is unsubstituted or substituted by a substituent OCF3; Rn+ is selected from the group consisting of H+, Li+, Na+, K+, Mg2+, Ca2+, Zn2+, Cu2+, Al3+, Ti3+, Fe2+, Fe3+, B3+, [N(R20)(R21)(R22)R23]+, and [P(R20)(R21)(R22)R23]+; R20, R21, R22 and R23 are identical or different and independently from each other selected from the group consisting of H, C1-8 alkyl, C5-6 cycloalkyl, phenyl, benzyl, vinyl and allyl; n is 1, 2 or 3; wherein the total content of the three components in MIXTURE-TRIPLE is of from 50 to 100%, the % being % by weight based on the total weight of MIXTURE-TRIPLE; wherein the relative ratio of the three components in MIXTURE-TRIPLE is of from 2 to 98% of the compound of formula (II), 49 to 1% of the compound of formula (III), and 49 to 1% of the compound of formula (IV); the % are % by weight and are based on the combined weight of the three components in MIXTURE-TRIPLE; the relative ratios of the three components add up to 100%. ### Claim 2 (depends on 1) The method according to claim 1, wherein X1 and X2 are identical or different and independently from each other selected from the group consisting of F, Cl, Br, RESF, and tolyl; Rn+ is selected from the group consisting of H+, Li+, Na+, K+, Mg2+, Al3+, and [N(R20)(R21)(R22)R23]+; R20, R21, R22 and R23 are identical or different and independently from each other selected from the group consisting of H, C1-4 alkyl, phenyl, benzyl, vinyl and allyl; n is 1, 2 or 3. ### Claim 3 (depends on 1) The method according to claim 1, wherein TEMP1-1 is from 80 to 300° C. ### Claim 4 (depends on 1) The method according to claim 1, wherein the total content of the three components in MIXTURE-TRIPLE is of from 75 to 100%, the % being % by weight based on the total weight of MIXTURE-TRIPLE. ### Claim 5 (depends on 1) The method according to claim 1, wherein the relative ratio of the three components in MIXTURE-TRIPLE is of from 2 to 96% of the compound of formula (II), 49 to 2% of the compound of formula (III), and 49 to 2% of the compound of formula (IV); the % are % by weight and are based on the combined weight of the three components in MIXTURE-TRIPLE; the relative ratios of the three components add up to 100%. ### Claim 6 (depends on 1) The method according to claim 1, wherein REAC1-1 is done in a continuous way. ### Claim 7 (depends on 1) The method according to claim 1, wherein STEP comprises two steps, a step STEP1-1 and a step STEP1-3; in STEP1-1 a mixture MIXTURE1-1 which is a mixture of MIXTURE-TRIPLE and HF, is heated in a device DEVICE1-1 to TEMP1-1, wherein REAC1-1 takes place in DEVICE-1 resulting in a reaction mixture, and in STEP1-3 the reaction mixture from DEVICE1-1 passes through a device DEVICE1-3, wherein DEVICE1-3 is a device for back pressure regulation. ### Claim 8 (depends on 7) The method according to claim 7, wherein STEP1 comprises a third step, a STEP1-2, which is done between STEP1-1 and STEP1-3, in STEP1-2 the reaction mixture from DEVICE1-1 passes through a DEVICE1-2 before passing through device DEVICE1-3, DEVICE1-2 is a device for cooling the reaction mixture. ### Claim 9 (depends on 7) The method according to claim 7, wherein the method comprises furthermore a step STEP1-4, STEP1-4 is done after STEP1-3, in STEP-4 the reaction mixture from DEVICE1-3 passes through a device DEVICE1-4, DEVICE1-4 is a device for separating gaseous components from liquid components in the reaction mixture. ### Claim 10 (depends on 1) The method according to claim 1, wherein MIXTURE-TRIPLE is prepared in a step STEP0; STEP0 is done before STEP1; STEP0 comprises a reaction REAC0-1; REAC0-1 is a reaction of the compound of formula (III) with the compound of formula (IV). ### Claim 11 (depends on 10) The method according to claim 10, wherein REAC0-1 is done at a temperature TEMP0-1, TEMP0-1 is from 180 to 300° C. ### Claim 12 (depends on 10) The method according to claim 10, wherein REAC0-1 is done in a continuous way. ### Claim 13 (depends on 10) The method according to claim 10, wherein STEP0 comprises a step STEP0-1; STEP0-1 comprises the reaction REAC0-1; in STEP0-1 a mixture MIXTURE0-1 of the compound of formula (III) and the compound of formula (IV) is heated in a DEVICE0-1 to a TEMP0-1, REAC0-1 takes place in DEVICE0-1 resulting in a reaction mixture. ### Claim 14 (depends on 13) The method according to claim 13, wherein STEP0 comprises another step STEP0-2; STEP0-2 is done after STEP0-1; in STEP0-2 the reaction mixture from DEVICE0-1 passes through a device DEVICE0-2, DEVICE0-2 is a device for cooling the reaction mixture. ### Claim 15 (depends on 10) The method according to claim 10, wherein REAC0-1 and REAC1-1 are done continuously and consecutively.