Sodium Hydroxide → HCID 21430465, compound

HRID 437171Notes

Reaction equation

HRID 437171 reaction equation
[CH2:1]([O:3][CH2:4][CH2:5][NH:6][S:7]([C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][C:18]=1[Cl:19])[C:13]([OH:15])=[O:14])(=[O:9])=[O:8])[CH3:2].[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.[OH-].[Na+]>O>[ClH:19].[ClH:19].[CH2:1]([O:3][CH2:4][CH2:5][NH:6][S:7]([C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][C:18]=1[N:24]1[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]1)[C:13]([OH:15])=[O:14])(=[O:9])=[O:8])[CH3:2]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 531671-MethylpiperazineHCID 21430481HCID 21430481, compound

Product 1

HCID 21430465HCID 21430465, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

31 Grams of 3-(2-ethoxyethylsulfamoyl)-4-chlorobenzoic acid and 30 g of N-methylpiperazine were heated for 4 hours at 140° C. Subsequently the excess base was eliminated in vacuo. The residue was dissolved in 0.2 l of water, and the solution was adjusted to a pH value of 9.5 by means of 2N NaOH. After evaporating the solution in vacuo, the residue was extracted with boiling ethanol, and the solution, which had been concentrated to 100 ml, was mixed with 100 ml of ethanolic HCl of 10% strength. After having been triturated and cooled, the final product crystallized within a short time and was dried at 60° C. after washing with ethanol.

Workup

  1. customAfter evaporating the solution in vacuo
  2. extractionthe residue was extracted with boiling ethanol
  3. concentrationthe solution, which had been concentrated to 100 ml
  4. additionwas mixed with 100 ml of ethanolic HCl of 10% strength
  5. customAfter having been triturated
  6. temperaturecooled
  7. customthe final product crystallized within a short time
  8. customwas dried at 60° C.
  9. washafter washing with ethanol

Sources & evidence

ORD record
ord-59d3c4fc6aac426fb2f6062d1aaf56aa
Source dataset
uspto-grants-1977_06
Patent number
US04029787

Reaction notes

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