Trifluoroacetic acid → HCID 57469137, 화합물

HRID 1989619노트

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HRID 1989619 반응식
C([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]2[N:16]=[CH:17][N:18]([C:20]3[CH:25]=[C:24]([CH3:26])[CH:23]=[C:22]([C:27]4[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=4)[N:21]=3)[CH:19]=2)[CH:10]=1)(=[O:8])=[O:7])(C)(C)C.C(O)(C(F)(F)F)=O>>[Cl:33][C:30]1[CH:31]=[CH:32][C:27]([C:22]2[N:21]=[C:20]([N:18]3[CH:19]=[C:15]([C:11]4[CH:10]=[C:9]([S:6]([NH2:5])(=[O:7])=[O:8])[CH:14]=[CH:13][CH:12]=4)[N:16]=[CH:17]3)[CH:25]=[C:24]([CH3:26])[CH:23]=2)=[CH:28][CH:29]=1

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 57469036HCID 57469036, 화합물

생성물 1

HCID 57469137HCID 57469137, 화합물수율 101.4%

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온도
23 °C

실험 절차

To N-tert-butyl-3-{1-[6-(4-chloro-phenyl)-4-methyl-pyridin-2-yl]-1H-imidazol-4-yl}-benzenesulfonamide (example 298) (0.028 g, 0.058 mmol) was added TFA (2 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 an off-white solid (0.025 g, 101%). MS (ISP) 425.1 [(M+H)+] and 427 [(M+2+H)+].

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-2f65ac2759684b63b1d27ea49953fd0e
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642264B2

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