Caldaret → 5-methyl-2-(1-piperazinyl)benzenesulfonic acid monohydrate

HRID 1603522Notes

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

Participants

3

Reactant 1

HCID 6433076Caldaret

Product 1

HCID 98169815-methyl-2-(1-piperazinyl)benzenesulfonic acid 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

  1. temperatureby heating a bath
  2. customisolated from outer air
  3. waitleft in the above plastic sheet housing
  4. additionThe crystals were occasionally dispersed
  5. customsweat formed on inner wall of the housing
  6. temperatureweight increase

Sources & evidence

ORD record
ord-4565e4f52f8a4ba590da7188f33c38f5
Source dataset
uspto-grants-1999_11
Patent number
US05990113

Reaction notes

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