Reaction equation
[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH2:5].[S:8](Cl)([OH:11])(=O)=[O:9].[CH:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(=O)([O-])[O-].[Na+].[Na+]>[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH:5][S:8]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:11])=[O:9]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
56 g 2-aminoacetaldehyde dimethyl acetal are dissolved in 200 ml of a 14 wt. % aqueous sodium carbonate solution at 20 ° C. in a three-necked flask, equipped with a thermometer, reflux condenser, tap funnel and magnetic stirrer. Subsequently, 88 g benzene sulfochloride are added drop-wise within 1 hour at this temperature under intensive stirring followed by another 2 hours of heating the reaction to 40° to 50° C. mixture under vigorous stirring. After that the intensive smell of benzene sulfochloride has disappeared and a second phase has formed. This heavy oily phase is separated in the separatory funnel, imbibed using diethyl ether and dried over water-free sodium sulfate. Once the drying agent has been removed and the ether has been distilled off, 112 g of the product are obtained (yield: 88 based on the amino acetal used).
Workup
- customequipped with a thermometer
- temperaturereflux condenser, tap funnel and magnetic stirrer
- temperatureof heating
- customthe reaction to 40° to 50° C. mixture under vigorous stirring
- customa second phase has formed
- customThis heavy oily phase is separated in the separatory funnel
- dry with materialdried over water-free sodium sulfate
- customOnce the drying agent has been removed
- distillationthe ether has been distilled off
Sources & evidence
- ORD record
- ord-0ae5ceb401a74070a80e1e70c4762bb6
- Source dataset
- uspto-grants-1997_12
- Patent number
- US05698360
Linked notes
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