반응 #922

ord-4d0fbf7c4db24ef2820d2d87a9754e6c

반응 방정식

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
수율 92.9%
CN(C)C(=O)c1c(S(N)(=O)=O)ccn1C
3 -(Aminosulfonyl)-N,N,1-trimethyl-1H-pyrrole-2-carboxamide
수율 92.9%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONThree portions of diethyl ether were added to the residue
  3. 3
    기타removed by evaporation
  4. 4
    기타to remove residual TFA

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723410uspto-grants-1998_03