Sulfuric Acid → HCID 22111842, compound
Reaction equation
[OH:1][S:2]([OH:5])(=O)=[O:3].[CH:6]([C:9]1[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=1[NH2:11])([CH3:8])[CH3:7]>O>[NH2:11][C:10]1[CH:12]=[CH:13][C:14]([S:2]([OH:5])(=[O:3])=[O:1])=[CH:15][C:9]=1[CH:6]([CH3:8])[CH3:7]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
5.7 ml of H2SO4 are added to 10 ml of water, the mixture is heated to 80° C. and 13.5 g of 2-isopropylaniline are then added. The water is evaporated off by heating under vacuum, and the temperature is then gradually raised over one and a half hours to reach 260° C. After 3 hours with stirring and under vacuum at 260° C., the reaction medium is allowed to return to RT and to atmospheric pressure, and is then heated for 30 minutes in the presence of 15 ml of NaOH and 100 ml of water in order to dissolve the reaction medium. The insoluble matter is filtered off, and the mixture is cooled to 5° C. and then acidified to pH 1 by adding concentrated H2SO4. The precipitate formed is filtered off, washed with 5 ml of cold water and dried to obtain 20 g of the expected product.
Workup
- customThe water is evaporated off
- temperatureby heating under vacuum
- temperaturethe temperature is then gradually raised over one and a half hours
- customto reach 260° C
- customto return to RT and to atmospheric pressure
- temperatureis then heated for 30 minutes in the presence of 15 ml of NaOH and 100 ml of water in order
- dissolutionto dissolve the reaction medium
- filtrationThe insoluble matter is filtered off
- temperaturethe mixture is cooled to 5° C.
- additionby adding concentrated H2SO4
- customThe precipitate formed
- filtrationis filtered off
- washwashed with 5 ml of cold water
- customdried
Sources & evidence
- ORD record
- ord-40511f7f6c0a4cc98fccb10377b54d69
- Source dataset
- uspto-grants-1999_07
- Patent number
- US05925661
Reaction notes
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