Sulfuric Acid → HCID 68720633, compound

HRID 1787953Notes

Reaction equation

HRID 1787953 reaction equation
[Na+].[CH3:2][C:3]1[CH:8]=[CH:7][C:6]([P:9]([C:12](=[O:19])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)(=[O:11])[O-:10])=[C:5]([CH3:20])[C:4]=1[CH3:21].S(=O)(=O)(O)O>O>[CH3:2][C:3]1[CH:8]=[CH:7][C:6]([P:9]([C:12](=[O:19])[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)(=[O:10])[OH:11])=[C:5]([CH3:20])[C:4]=1[CH3:21]

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 131727372HCID 131727372, compound

Product 1

HCID 68720633HCID 68720633, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

401.55 g of the sodium salt from Example 1 were dissolved in 1500 ml of water acidified to pH 1 with 1300 ml of 0.5 molar sulfuric acid. After 1 hour, the crystal batch which had precipitated was filtered off with suction, washed twice with 700 ml of water each time and sucked dry. The filter cake was dried azeotropically with 1500 ml of toluene in a water separator. The clear, pale-yellow toluene solution was evaporated at 50° C., and the acid was recrystallized from 2150 ml of ethyl acetate. The crystals were filtered off with suction at 0°, washed with ethyl acetate and dried at 60° C. under reduced pressure. Weight: 300 g (80% of theory) of pale-yellow crystals.

Workup

  1. customthe crystal batch which had precipitated
  2. filtrationwas filtered off with suction
  3. washwashed twice with 700 ml of water each time
  4. customsucked dry
  5. dry with materialThe filter cake was dried azeotropically with 1500 ml of toluene in a water separator
  6. customThe clear, pale-yellow toluene solution was evaporated at 50° C.
  7. customthe acid was recrystallized from 2150 ml of ethyl acetate
  8. filtrationThe crystals were filtered off with suction at 0°
  9. washwashed with ethyl acetate
  10. customdried at 60° C. under reduced pressure

Sources & evidence

ORD record
ord-035e490eb66b4793b511ec5eb9352753
Source dataset
uspto-grants-2009_03
Patent number
US07511084B2

Reaction notes

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