Trifluoroacetic acid → 5-[4-(3-Methoxy-4-trifluoromethyl-phenyl)-6-methyl-[2,4']bipyridinyl-2'-yl]-thiophene-2-sulfonic acid amide

HRID 1989650노트

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HRID 1989650 반응식
C([NH:5][S:6]([C:9]1[S:10][C:11]([C:14]2[CH:19]=[C:18]([C:20]3[CH:25]=[C:24]([C:26]4[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[C:28]([O:36][CH3:37])[CH:27]=4)[CH:23]=[C:22]([CH3:38])[N:21]=3)[CH:17]=[CH:16][N:15]=2)=[CH:12][CH:13]=1)(=[O:8])=[O:7])(C)(C)C.C(O)(C(F)(F)F)=O>>[CH3:37][O:36][C:28]1[CH:27]=[C:26]([C:24]2[CH:23]=[C:22]([CH3:38])[N:21]=[C:20]([C:18]3[CH:17]=[CH:16][N:15]=[C:14]([C:11]4[S:10][C:9]([S:6]([NH2:5])(=[O:7])=[O:8])=[CH:13][CH:12]=4)[CH:19]=3)[CH:25]=2)[CH:31]=[CH:30][C:29]=1[C:32]([F:35])([F:33])[F:34]

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 247599495-[4-(3-Methoxy-4-trifluoromethyl-phenyl)-6-methyl-[2,4']bipyridinyl-2'-yl]-thiophene-2-sulfonic acid tert-butylamide

생성물 1

HCID 247599515-[4-(3-Methoxy-4-trifluoromethyl-phenyl)-6-methyl-[2,4']bipyridinyl-2'-yl]-thiophene-2-sulfonic acid amide수율 100%

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온도
23 °C

실험 절차

To 5-[4-(3-methoxy-4-trifluoromethyl-phenyl)-6-methyl-[2,4′]bipyridinyl-2′-yl]-thiophene-2-sulfonic acid tert-butylamide (example 339) (0.100 g, 0.178 mmol) was added TFA (3 mL) and the reaction mixture was stirred at 23° C. for 16 h. The mixture was evaporated to dryness and partitioned between EtOAc and saturated NaHCO3 solution, the organic layer was dried over Na2SO4. Removal of the solvent in vacuum left a crude product which was triturated with diethyl ether to give the title compound as a white solid (0.090 g, 100%). MS (ISP) 506.2 [(M+H)+]; mp 261° C. (dec.).

후처리

  1. customThe mixture was evaporated to dryness
  2. custompartitioned between EtOAc and saturated NaHCO3 solution
  3. dry with materialthe organic layer was dried over Na2SO4
  4. customRemoval of the solvent in vacuum
  5. waitleft a crude product which
  6. customwas triturated with diethyl ether

출처 및 근거

ORD 기록
ord-099fbf821c984e15a4362a073695d400
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642264B2

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