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Caldaret → Caldaret monohydrate

HRID 1603522
Notes
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Reaction equation

HRID 1603522 reaction equation
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[C:6]([S:8]([OH:11])(=[O:10])=[O:9])[CH:7]=1>O>[OH2:9].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[C:6]([S:8]([OH:11])(=[O:9])=[O:10])[CH:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 6433076Caldaret

Product 1

HCID 9816981Caldaret monohydrate

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Steam was generated by heating a bath filled with water at 50° C. in a plastic sheet housing isolated from outer air. The anhydrous crystal of 5-Methyl-2-(1-piperazinyl)benzenesulfonic acid (4886.16 g) prepared by the method described in the Japanese Patent Unexamined Publication (KOKAI) No.(Hei)3-7263/1991 was spread in a stainless flat container and left in the above plastic sheet housing. The crystals were occasionally dispersed and sweat formed on inner wall of the housing and the stainless container was wiped. After 22.5 hours, weight increase ceased and 5217.65 g in total of 5-methyl-2-(1-piperazinyl)benzenesulfonic acid monohydrate was obtained as white crystals. The result of the elemental analysis verified that the crystals were the monohydrate crystals.

Workup

  • temperatureby heating a bath
  • customisolated from outer air
  • waitleft in the above plastic sheet housing
  • additionThe crystals were occasionally dispersed
  • customsweat formed on inner wall of the housing
  • temperatureweight increase
  • Sources & evidence

    ORD record
    ord-4565e4f52f8a4ba590da7188f33c38f5
    Source dataset
    uspto-grants-1999_11
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US05990113

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes