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

HRID 1066714Notes

Reaction equation

HRID 1066714 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-ea7d8945e73c42158b847348183f756d
Source dataset
uspto-grants-2001_06
Patent number
US06245767B1

Reaction notes

Loading…