反应 #918

ord-0d13730de7524a88a677102766469c81

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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