Trifluoroacetic acid → 2-Bromo-1-methyl-1H-pyrrole-3-sulfonamide

HRID 2259183

反応式

HRID 2259183 の反応式
[Br:1][C:2]1[N:3]([CH3:15])[CH:4]=[CH:5][C:6]=1[S:7]([NH:10]C(C)(C)C)(=[O:9])=[O:8].C(O)(C(F)(F)F)=O>C(Cl)Cl>[Br:1][C:2]1[N:3]([CH3:15])[CH:4]=[CH:5][C:6]=1[S:7]([NH2:10])(=[O:8])=[O:9]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 196938302-bromo-N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide

生成物 1

HCID 196938442-Bromo-1-methyl-1H-pyrrole-3-sulfonamide収率 21.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7.11 g (24 mmol) of 2-bromo-N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 50 mL methylene chloride under a nitrogen atmosphere was added 50 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 crude residue and was removed by evaporation to remove residual TFA, which yielded 1.23 g of the title compound as a light brown solid. 1H NMR (Acetone-d6, 200 MHz.) δ: 7.36(d,1H), 6.49(d,1H), 6.3(bs,2H) 3.68(s,3H).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionThree portions of diethyl ether were added to the crude residue
  3. customwas removed by evaporation
  4. customto remove residual TFA, which

出典と根拠

ORDレコード
ord-24fca5966e304194948bc21b192c7f7a
出典データセット
uspto-grants-1995_12
特許番号
US05472933

関連ノート

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