Reaktionsgleichung
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[Br:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[S:16]([NH2:19])(=[O:18])=[O:17].CN(C=O)C.S([O-])(O)(=O)=O.[Na+].O>>[Br:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[S:16](/[N:19]=[CH:3]/[N:4]([CH3:6])[CH3:5])(=[O:18])=[O:17]Komponenten
6
Versuchsvorschrift
1,1-Dimethoxy-N,N-dimethylmethanamine (14.6 mL, 104 mmol) was added to a solution of 2-bromobenzene-1-sulfonamide (20.4 g, 86.4 mmol) in DMF (56 mL, 720 mmol) and the resulting solution was stirred at room temperature for 90 minutes. A solution of sodium hydrogen sulfate (1.7 g, 14 mmol) in water (170 mL, 9.4 mol) was cooled at 0° C. and then added to the reaction mixture. The precipitate was filtered, washed with water, and dried to yield the title compound (24.3 g) as a white solid.
Aufarbeitung
- additionadded to the reaction mixture
- filtrationThe precipitate was filtered
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-3ab83d03f7e8477f94094926eaa09f41
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08822522B2
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