Trifluoroacetic acid → 3-(Aminosulfonyl)-N,N,1-trimethyl-1H-pyrrole-2-carboxamide

HRID 2259189

反応式

HRID 2259189 の反応式
CC([NH:5][S:6]([C:9]1[CH:13]=[CH:12][N:11]([CH3:14])[C:10]=1[C:15]([N:17]([CH3:19])[CH3:18])=[O:16])(=[O:8])=[O:7])(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:5][S:6]([C:9]1[CH:13]=[CH:12][N:11]([CH3:14])[C:10]=1[C:15]([N:17]([CH3:19])[CH3:18])=[O:16])(=[O:8])=[O:7]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 196938293-[[(1,1-dimethylethyl)amino]sulfonyl]N,N,1-trimethyl-1H-pyrrole-2-carboxamide

生成物 1

HCID 196938183-(Aminosulfonyl)-N,N,1-trimethyl-1H-pyrrole-2-carboxamide収率 92.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

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. 1H NMR(Me2SO-d6, 200 MHz.) δ: 6.99(bs,2H), 6.88(d,1H), 6.34(d,1H), 3.47(s,3H), 2.96(s,3H), 2.81(s,3H).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionThree portions of diethyl ether were added to the residue
  3. customremoved by evaporation
  4. customto remove residual TFA

出典と根拠

ORDレコード
ord-c7fb2f6b0ce54c51964100c3d03d00cd
出典データセット
uspto-grants-1995_12
特許番号
US05472933

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