Hydrochloric Acid → HCID 15057634, compound

HRID 654024Notes

Reaction equation

HRID 654024 reaction equation
[OH:1][CH:2]([CH:26]1[CH2:30][O:29]C(C)(C)[O:27]1)[CH2:3][NH:4][C:5](=[O:25])[C:6]1[CH:11]=[CH:10][C:9]([S:12](=[O:24])(=[O:23])[NH:13][C:14]2[C:19]([F:20])=[CH:18][C:17]([F:21])=[CH:16][C:15]=2[F:22])=[CH:8][CH:7]=1.Cl>C(O)C.O>[OH:1][CH:2]([CH:26]([OH:27])[CH2:30][OH:29])[CH2:3][NH:4][C:5](=[O:25])[C:6]1[CH:7]=[CH:8][C:9]([S:12](=[O:23])(=[O:24])[NH:13][C:14]2[C:19]([F:20])=[CH:18][C:17]([F:21])=[CH:16][C:15]=2[F:22])=[CH:10][CH:11]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 15057633HCID 15057633, compound

Product 1

HCID 15057634HCID 15057634, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

4.74 g (10 mmol) of 4-[N-(2,4,6-trifluorophenyl)sulfamoyl]- benzoic acid-[2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamide] is dissolved in a mixture of 50 ml of ethanol and 20 ml of water and the solution is acidified to pH 1 with dilute hydrochloric acid. It is stirred at this pH for 4 hours at 60° C. The solution is then adjusted to pH 6.3 with 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. 3.4 g (7.83 mmol)=78.3% 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. custom3.4 g (7.83 mmol)=78.3% of the theoretical yield
  5. customis obtained as an amorphous solid

Sources & evidence

ORD record
ord-b7c569c52bd84e78acceec5f2cf3c1f5
Source dataset
uspto-grants-1992_07
Patent number
US05130119

Reaction notes

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