反応 #920

ord-bce13e6e0f2b4556bf712059577ecdcd

反応方程式

CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C
(1,1-dimethylethyl)-N2,N2,1-trimethyl-1H-pyrrole-2,3-disulfonamide
O=C(O)C(F)(F)F
TFA
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)ccn1C
title compound
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)ccn1C
N2,N2,1-Trimethyl-1H-pyrrole-2,3-disulfonamide

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONThree portions of diethyl ether were added to the solid residue
  3. 3
    その他removed by evaporation
  4. 4
    その他to remove residual TFA
  5. 5
    ろ過filtered

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.

出典

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