Hydrochloric Acid → HCID 15057638, compound

HRID 654027Notes

Reaction equation

HRID 654027 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][CH:9]=[C:8]([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: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:11]=[CH:10][CH:9]=[C:8]([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:7]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 15057637HCID 15057637, compound

Product 1

HCID 15057638HCID 15057638, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

4.74 g (10 mmol) of 3-[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. At this pH, it is stirred for 4 hours at 60° C. The solution is then adjusted to pH 6.6 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. 3.61 g (8.32 mmol)=83.2% 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. custom3.61 g (8.32 mmol)=83.2% of the theoretical yield
  5. customis obtained as an amorphous solid

Sources & evidence

ORD record
ord-dbed7cd0939a47c999129e88202a8482
Source dataset
uspto-grants-1992_07
Patent number
US05130119

Reaction notes

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