Hydrochloric Acid → HCID 15057613, compound

HRID 654015Notes

Reaction equation

HRID 654015 reaction equation
[OH:1][CH:2]([CH:41]1[CH2:45][O:44]C(C)(C)[O:42]1)[CH2:3][NH:4][C:5](=[O:40])[C:6]1[CH:24]=[C:23]([S:25](=[O:39])(=[O:38])[NH:26][C:27]2[CH:32]=[CH:31][C:30]([F:33])=[CH:29][C:28]=2[C:34]([F:37])([F:36])[F:35])[CH:22]=[C:8]([C:9]([NH:11][CH2:12][CH:13]([OH:21])[CH:14]2[CH2:18][O:17]C(C)(C)[O:15]2)=[O:10])[CH:7]=1.Cl>C(O)C.O>[OH:1][CH:2]([CH:41]([OH:42])[CH2:45][OH:44])[CH2:3][NH:4][C:5](=[O:40])[C:6]1[CH:24]=[C:23]([S:25](=[O:38])(=[O:39])[NH:26][C:27]2[CH:32]=[CH:31][C:30]([F:33])=[CH:29][C:28]=2[C:34]([F:37])([F:35])[F:36])[CH:22]=[C:8]([C:9]([NH:11][CH2:12][CH:13]([OH:21])[CH:14]([OH:15])[CH2:18][OH:17])=[O:10])[CH:7]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 15057612HCID 15057612, compound

Product 1

HCID 15057613HCID 15057613, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

3.79 g (5.46 mmol) of 5-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-isophthalic acid-bis[2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamide] is dissolved in a mixture of 40 ml of ethanol and 10 ml of water and the solution is acidified with dilute hydrochloric acid to pH 1. It is stirred at this pH for 4 hours at 60° C. The solution is then adjusted to pH 6.1 with the anion exchanger Amberlite IRA 67, filtered and evaporated to dryness in a vacuum. The solid amorphous residue is dried in a vacuum at 50° C. 2.55 g (4.16 mmol) =76.12% of the theoretical yield is obtained as an amorphous solid.

Workup

  1. filtrationfiltered
  2. customevaporated to dryness in a vacuum
  3. customThe solid amorphous residue is dried in a vacuum at 50° C
  4. custom2.55 g (4.16 mmol) =76.12% of the theoretical yield
  5. customis obtained as an amorphous solid

Sources & evidence

ORD record
ord-698dcb67534747ff8e4e5d6eeaf3f9ff
Source dataset
uspto-grants-1992_07
Patent number
US05130119

Reaction notes

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