反応 #911

ord-740719404b1e4815a4a77e34574adcd7

反応方程式

COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
methyl 3-[[(1,1-dimethylethyl)amino]-sulfonyl]-1-methyl-1H-pyrrole-2-carboxylate
O=C(O)C(F)(F)F
trifluoroacetic acid
COC(=O)c1c(S(N)(=O)=O)ccn1C
title compound
COC(=O)c1c(S(N)(=O)=O)ccn1C
Methyl 3-(aminosulfonyl)-1-methyl-1H-pyrrole-2-carboxylate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The gold solution was concentrated to an oily residue
  2. 2
    workup.ADDITIONDiethyl ether was added to the 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 3.53 g of methyl 3-[[(1,1-dimethylethyl)amino]-sulfonyl]-1-methyl-1H-pyrrole-2-carboxylate in 40 mL, of methylene chloride under an nitrogen atmosphere was added 80 mL of trifluoroacetic acid (TFA). The gold solution was stirred at room temperature overnight ca. 16 hours. The gold solution was concentrated to an oily residue. Diethyl ether was added to the residue and removed by evaporation to remove residual TFA. The resulting solid was suspended in diethyl ether and filtered affording the title compound as a tan solid, m.p. 105°-107° C.

出典

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