Acetone → HCID 87597198, compound

HRID 514691Notes

Reaction equation

HRID 514691 reaction equation
CC(C)=[O:3].[C:5]1([S:11]([OH:14])(=[O:13])=[O:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.O>>[OH2:3].[S:11]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([OH:14])(=[O:13])=[O:12].[S:11]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([OH:14])(=[O:13])=[O:12]

Participants

4

Reactant 3

HCID 180Acetone2×HCID 962WaterHCID 7371Benzenesulfonic Acid

Product 1

HCID 87597198HCID 87597198, compound

Procedure

Approximately 3 mL of acetone was added to ca. 500 mg of Compound 1 to form a slurry. In a separate vial, ca. 1 mL of acetone was added to 2 equivalents of benzenesulfonic acid in order to dissolve the acid. The acid solution was then added in small aliquots to the freebase slurry while stirring. The reaction was stirred for ca. 1 day while temperature cycling between 0 and ambient temperature (ca. 22° C.). After 1 day, deionized water was added to the reaction mixture and the slurry was allowed to stir for ca. 3 hours before being isolated and dried at ambient under vacuum.

Workup

  1. customto form a slurry
  2. dissolutionto dissolve the acid
  3. additionThe acid solution was then added in small aliquots to the freebase slurry
  4. stirringThe reaction was stirred for ca. 1 day while temperature cycling between 0 and ambient temperature (ca. 22° C.)
  5. additionwas added to the reaction mixture
  6. stirringto stir for ca. 3 hours
  7. custombefore being isolated
  8. customdried at ambient under vacuum

Sources & evidence

ORD record
ord-77441b7842054257997fbbcbd78e2222
Source dataset
uspto-grants-2015_08
Patent number
US09108927B2

Reaction notes

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