Ethanol → 5-methyl-2-(1-piperazinyl)benzenesulfonic acid monohydrate
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.C(O)C>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]=1Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 5 °C
Procedure
The anhydrous crystal of 5-Methyl-2-(1-piperazinyl)benzenesulfonic acid (10.00 g) and ethanol containing 50% (V/V) water (80 ml) were added in a 200 ml round-bottomed flask and the crystals were thoroughly dissolved by heating under reflux with stirring. The solution was then cooled to 5° C. with stirring and stirring was further continued for 2 hours at the same temperature. The precipitated crystals were collected by suction filtration and washed with ethanol containing 50% (V/V) water (20 ml). The crystals obtained were dried at 50° C. under 90 mmHg for 3 hours to give 5-methyl-2-(1-piperazinyl)benzenesulfonic acid monohydrate as white crystals (9.49 g, yield: 88.7%). After drying was further continued for 27 hours under the same conditions, the weight and the appearance of the monohydrate were not changed. Water content measured by a Karl Fischer water content meter was 6.74%, which further verified that the product was the monohydrate.
Workup
- dissolutionthe crystals were thoroughly dissolved
- temperatureby heating
- temperatureunder reflux
- stirringwith stirring
- stirringstirring
- filtrationThe precipitated crystals were collected by suction filtration
- washwashed with ethanol containing 50% (V/V) water (20 ml)
- customThe crystals obtained
- customwere dried at 50° C. under 90 mmHg for 3 hours
Sources & evidence
- ORD record
- ord-8a547f0b03d340a999e858a28eb2d8bd
- Source dataset
- uspto-grants-1999_11
- Patent number
- US05990113
Reaction notes
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