Hydrochloric Acid → HCID 22609743, compound
Reaction equation
[CH3:1][S:2]([CH:5]=[CH2:6])(=[O:4])=[O:3].[CH3:7][NH2:8].[ClH:9]>C(O)C>[ClH:9].[CH3:7][NH:8][CH2:6][CH2:5][S:2]([CH3:1])(=[O:4])=[O:3]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Methylvinyl sulphone (2.1 g, 19.78 mmol) and methylamine (33% solution in IMS, 40 ml , excess) were mixed and heated at reflux under a nitrogen atmosphere for 6 hours. After standing overnight at room temperature, the mixture was concentrated in vacuo to give a yellow oil, which was treated with ethereal HCl to give a sticky solid. Trituration with absolute ethanol gave the title compound as a white solid which was collected by filtration and dried at 60° C. in vacuo (1.01 g, 5.82 mmol, 29%); δH [2H6]DMSO 9.27 (2H, br s), 3.59 (2H, dd), 3.31 (2H, dd), 3.12 (3H, s), 2.57 (3H, s).
Workup
- temperatureheated
- temperatureat reflux under a nitrogen atmosphere for 6 hours
- concentrationthe mixture was concentrated in vacuo
- customto give a yellow oil, which
- customto give a sticky solid
Sources & evidence
- ORD record
- ord-36a2c29b2bad4d1f9f8a1c491c6c1464
- Source dataset
- uspto-grants-2004_12
- Patent number
- US06828320B2
Reaction notes
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