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

HRID 2259189

반응식

HRID 2259189 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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. 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).

후처리

  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

출처 및 근거

ORD 기록
ord-c7fb2f6b0ce54c51964100c3d03d00cd
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05472933

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