反応 #922

ord-4d0fbf7c4db24ef2820d2d87a9754e6c

反応方程式

CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
3-[[(1,1-dimethylethyl)amino]sulfonyl]-N,N,1-trimethyl-1H-pyrrole-2-carboxamide
O=C(O)C(F)(F)F
TFA
CN(C)C(=O)c1c(S(N)(=O)=O)ccn1C
title compound
収率 92.9%
CN(C)C(=O)c1c(S(N)(=O)=O)ccn1C
3 -(Aminosulfonyl)-N,N,1-trimethyl-1H-pyrrole-2-carboxamide
収率 92.9%

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 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 5.63 g of 3-[[(1,1-dimethylethyl)amino]sulfonyl]-N,N,1-trimethyl-1H-pyrrole-2-carboxamide in 75 mL of methylene chloride 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 residue and removed by evaporation to remove residual TFA, affording 4.21 g of the title compound as a gray solid, m.p. 185°-190.5° C.

出典

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