反応 #918

ord-0d13730de7524a88a677102766469c81

反応方程式

CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C
N-(1,1-dimethylethyl)-2-[(methoxyimino)-methyl]-1H-pyrrole-3-sulfonamide
O=C(O)C(F)(F)F
TFA
CON=Cc1c(S(N)(=O)=O)ccn1C
title compound
CON=Cc1c(S(N)(=O)=O)ccn1C
2-[(Methoxyimino)methyl]-1-methyl-1H-pyrrole-3-sulfonamide

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The orange reaction mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONThree portions of diethyl ether were added to the residue
  3. 3
    その他removed by evaporation
  4. 4
    その他to remove residual TFA

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723410uspto-grants-1998_03