Trifluoroacetic acid → 2-[(Methoxyimino)methyl]-1-methyl-1H-pyrrole-3-sulfonamide

HRID 2259186

反応式

HRID 2259186 の反応式
CC([NH:5][S:6]([C:9]1[CH:13]=[CH:12][NH:11][C:10]=1[CH:14]=[N:15][O:16][CH3:17])(=[O:8])=[O:7])(C)C.[C:18](O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:17][O:16][N:15]=[CH:14][C:10]1[N:11]([CH3:18])[CH:12]=[CH:13][C:9]=1[S:6]([NH2:5])(=[O:7])=[O:8]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 136144806N-(1,1-Dimethylethyl)-2-[(methoxyimino)methyl]-1H-pyrrole-3-sulfonamide

生成物 1

HCID 541233872-[(Methoxyimino)methyl]-1-methyl-1H-pyrrole-3-sulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5.74 g (21.9 mmol) of N-(1,1-dimethylethyl)-2-[(methoxyimino)-methyl]-1H-pyrrole-3-sulfonamide in 75 mL methylene chloride under a nitrogen atmosphere was add 75 mL of TFA. The clear orange reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The orange reaction mixture was concentrated in vacuo. Three portions of diethyl ether were added to the residue and removed by evaporation to remove residual TFA, affording 3.49 g of the title compound as a gray solid, m.p. 120°-122° C. 1H NMR (CDCl3, 200 MHz.) δ: 8.43(s,1H), 6.66(d,1H), 6.54(d,1H), 6.1-6.7(bs,2H), 3.96(s,3H), 3.79(s,3H).

後処理

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

出典と根拠

ORDレコード
ord-930b5ef0b22146469e59a8c1895f49b3
出典データセット
uspto-grants-1995_12
特許番号
US05472933

関連ノート

読み込み中…