Lithium Hydroxide → HCID 86688866, compound

HRID 1849951Notes

Reaction equation

HRID 1849951 reaction equation
C[O:2][C:3](=[O:11])[C:4]([F:10])([F:9])[S:5](F)(=[O:7])=[O:6].[Li+:12].[OH-:13]>O>[F:9][C:4]([F:10])([S:5]([OH:13])(=[O:7])=[O:6])[C:3]([O-:2])=[O:11].[Li+:12]

Participants

4

Reactant 2

HCID 3939Lithium HydroxideHCID 547667Methyl 2,2-difluoro-2-(fluorosulfonyl)acetate

Product 1

HCID 86688866HCID 86688866, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

In the first step, methyl-2,2-difluoro-2-(fluorosulfonyl)acetate (56.6 g, 0.29 mol) was added dropwise to an aqueous solution of 23.1 g (0.96 mol) LiOH in 200 mL of water at 0° C. After completing the addition, the reaction mixture was warmed gradually to room temperature and then heated to reflux for 16 h. The mixture was cooled to room temperature and insoluble inorganic salts were removed by filtration. The filtrate was acidified by slow addition of 5N HCl to a pH of 1. Water was distilled off and the crude product was dried under reduced pressure to produce the product lithium difluorosulfoacetate as crude and white waxy solid.

Workup

  1. additionthe addition
  2. temperatureheated
  3. temperatureto reflux for 16 h
  4. temperatureThe mixture was cooled to room temperature
  5. custominsoluble inorganic salts were removed by filtration
  6. additionThe filtrate was acidified by slow addition of 5N HCl to a pH of 1
  7. distillationWater was distilled off
  8. dry with materialthe crude product was dried under reduced pressure

Sources & evidence

ORD record
ord-881c256fdea343e9b7978d2bbc420000
Source dataset
uspto-grants-2015_02
Patent number
US08956799B2

Reaction notes

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