Trifluoroacetic acid → N2,N2,1-Trimethyl-1H-pyrrole-2,3-disulfonamide

HRID 2259187

반응식

HRID 2259187 반응식
CC([C:5]1[C:6]([S:17]([NH2:20])(=[O:19])=[O:18])=[C:7]([S:11]([N:14]([CH3:16])[CH3:15])(=[O:13])=[O:12])[N:8]([CH3:10])[CH:9]=1)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:15][N:14]([CH3:16])[S:11]([C:7]1[N:8]([CH3:10])[CH:9]=[CH:5][C:6]=1[S:17]([NH2:20])(=[O:19])=[O:18])(=[O:12])=[O:13]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 86749133(1,1-dimethylethyl)N2,N2,1-trimethyl-1H-pyrrole-2,3-disulfonamide

생성물 1

HCID 53663278N2,N2,1-Trimethyl-1H-pyrrole-2,3-disulfonamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionThree portions of diethyl ether were added to the solid residue
  3. customremoved by evaporation
  4. customto remove residual TFA
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-4dd314210e704fc987649daff1340a73
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05472933

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