Reaktion #2346369

Reaktionsgleichung

(1,1-dimethylethyl)N2,N2,1-trimethyl-1H-pyrrole-2,3-disulfonamide

TFA

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title compound

N2,N2,1-Trimethyl-1H-pyrrole-2,3-disulfonamide

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated in vacuo
2. 2
   workup.ADDITIONThree portions of diethyl ether were added to the solid residue
3. 3
   Sonstigeremoved by evaporation
4. 4
   Sonstigeto remove residual TFA
5. 5
   Filtrationfiltered

Vorschrift

To a solution of 6.95 g (21 mmol) of N3 -(1,1-dimethylethyl)N2,N2,1-trimethyl-1H-pyrrole-2,3-disulfonamide in 75 mL of methylene chloride under a nitrogen atmosphere was added 75 mL of TFA. The reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The reaction mixture was concentrated in vacuo. Three portions of diethyl ether were added to the solid residue and removed by evaporation to remove residual TFA. The solids were suspended in diethyl ether and filtered to yield 4.52 g of the title compound as a solid, m.p. 146°-148° C. 1H NMR (Acetone-d6, 200 MHz.) δ: 7.1(d,1H), 6.59(d,1H), 6.28(bs,2H), 3.95(s,3H), 2.93(s,6H).

Quelle