1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: C4F9SO2N(H)C4H8SO3Li was prepared essentially according to the procedure described in Preparation 3 replacing C4F9SO2NH(C2H4OH) with C4F9SO2NH2 (15.0 g; 0.05 moles), and the corresponding amounts of the following were used: LiOH—H2O (2.32 g; 0.055 moles), MTBE (100 mL), DME (100 mL), and 1,4-butanesultone (7.5 g; 0.055 moles). A waxy white solid was isolated (1.57 g; 7% yield). A waxy white solid was isolated (1.57 g; 7% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: C4F9SO2N(H)C4H8SO3Li was prepared essentially according to the procedure described in Preparation 3 replacing C4F9SO2NH(C2H4OH) with C4F9SO2NH2 (15.0 g; 0.05 moles), and the corresponding amounts of the following were used: LiOH—H2O (2.32 g; 0.055 moles), MTBE (100 mL), DME (100 mL), and 1,4-butanesultone (7.5 g; 0.055 moles). A waxy white solid was isolated (1.57 g; 7% yield). A waxy white solid was isolated (1.57 g; 7% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: C4F9SO2N(H)C4H8SO3Li was prepared essentially according to the procedure described in Preparation 3 replacing C4F9SO2NH(C2H4OH) with C4F9SO2NH2 (15.0 g; 0.05 moles), and the corresponding amounts of the following were used: LiOH—H2O (2.32 g; 0.055 moles), MTBE (100 mL), DME (100 mL), and 1,4-butanesultone (7.5 g; 0.055 moles). A waxy white solid was isolated (1.57 g; 7% yield). A waxy white solid was isolated (1.57 g; 7% yield)

反応条件: temp:98.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 1 L 3-necked round bottom flask equipped with a mechanical stirrer, thermocouple, reflux condenser and heating mantle was charged with C4F9SO2NH2 (58 g; 0.20 moles; as prepared above), NaOH (8.7 g; 0.22 moles; pellets) and water (60 mL) and heated at 98° C. for 45 minutes. Upon cooling to 76° C., ClCH2CO2Na (25 g; 0.22 moles, Sigma-Aldrich) was added and the temperature was then increased to 100° C. and maintained for 18 hours. Water was then added (200 mL) and a white solid appeared. The upper liquid phase was decanted off and discarded leaving the white solid, to which water (250 mL) was added. Water was removed to yield C4F9SO2N(H)CH2CO2Na (53.1 g ; 74% yield). A 1 L 3-necked round bottom flask equipped with a mechanical stirrer thermocouple, reflux condenser heating mantle Upon cooling to 76° C. the temperature was then increased to 100° C. maintained for 18 hours The upper liquid phase was decanted off discarded leaving the white solid Water was removed