Reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[S:10](Cl)(=[O:12])=[O:11].S([O-])([O-])=O.[Na+].[Na+].[C:20](=O)(O)[O-].[Na+].BrCC(O)=O>O>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[S:10]([CH3:20])(=[O:12])=[O:11]Participants
6
Conditions
- Temperature
- 150 °C
Procedure
2-Chloro-4,5-difluorobenzenesulfonyl chloride (300 mg) was added to a solution of sodium sulfite (306 mg) and sodium bicarbonate (153 mg) in water (4 mL). The mixture was heated to 150° C. in a sealed microwave vial for 400 seconds and allowed to cool. The mixture was treated with bromoacetic acid (253 mg) in water (1 mL), and heated to 150° C. for 300 seconds then allowed to cool, following which the precipitate was removed by filtration and dried in vacuo to give the desired compound (132 mg). The material was used without further purification.
Workup
- temperatureto cool
- temperatureheated to 150° C. for 300 seconds
- temperatureto cool
- customwas removed by filtration
- customdried in vacuo
Sources & evidence
- ORD record
- ord-b692961d75f642889f4ac786d8c9eff8
- Source dataset
- uspto-grants-2010_06
- Patent number
- US07745475B2
Linked notes
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