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

HRID 2259187

反応式

HRID 2259187 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4dd314210e704fc987649daff1340a73
出典データセット
uspto-grants-1995_12
特許番号
US05472933

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