Lithium hydroxide, monohydrate → HCID 178506957, compound

HRID 1792988Notes

Reaction equation

HRID 1792988 reaction equation
F[S:2]([C:5]([C:8]([C:11]([C:14]([O:17][C:18]([C:24]([O:27][CH3:28])([F:26])[F:25])([C:20]([F:23])([F:22])[F:21])[F:19])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])(=[O:4])=[O:3].[OH2:29].[OH-].[Li+:31]>O>[S:2]([C:5]([C:8]([C:11]([C:14]([O:17][C:18]([C:24]([O:27][CH3:28])([F:26])[F:25])([C:20]([F:23])([F:22])[F:21])[F:19])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([O:29][Li:31])(=[O:4])=[O:3]

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 131725866HCID 131725866, compound

Product 1

HCID 178506957HCID 178506957, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
75 °C

Procedure

A 250 mL round bottom flask was charged with FSO2(CF2)4OCF(CF3)CF2OCH3 (23.3 g, 0.048 mole) deionized water (150 g) and lithium hydroxide monohydrate (4.08 g, 0.097 mole). The resulting mixture was heated at 75° C. for about 18 hours, filtered and the aqueous solution treated with 48% aqueous HF until slightly acidic to pH paper. Water was removed using a rotary evaporator. The solid residue was treated with ethyl alcohol (about 200 mL; contained ˜5% isopropyl alcohol) and this mixture heated to reflux for two hours. The alcohol solution was filtered and the solvent removed by using a rotary evaporator to yield LiO3S(CF2)4OCF(CF3)CF2OCH3.

Workup

  1. filtrationfiltered
  2. additionthe aqueous solution treated with 48% aqueous HF until slightly acidic
  3. customWater was removed
  4. customa rotary evaporator
  5. additionThe solid residue was treated with ethyl alcohol (about 200 mL; contained ˜5% isopropyl alcohol)
  6. temperaturethis mixture heated
  7. temperatureto reflux for two hours
  8. filtrationThe alcohol solution was filtered
  9. customthe solvent removed
  10. customa rotary evaporator

Sources & evidence

ORD record
ord-478b6b6e95b94ca99e9f4c125d01b3e1
Source dataset
uspto-grants-2006_07
Patent number
US07078444B2

Reaction notes

Loading…