반응 #2346369

반응 방정식

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

TFA

→

title compound

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

용매

methylene chloride

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated in vacuo
2. 2
   workup.ADDITIONThree portions of diethyl ether were added to the solid residue
3. 3
   기타removed by evaporation
4. 4
   기타to remove residual TFA
5. 5
   여과filtered

실험 절차

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).

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