Trifluoroacetic acid → 4-Methyl-2-{1-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-1H-imidazol-4-yl}-thiazole-5-sulfonic acid amide

HRID 1989601노트

반응식

HRID 1989601 반응식
C([NH:5][S:6]([C:9]1[S:13][C:12]([C:14]2[N:15]=[CH:16][N:17]([C:19]3[CH:24]=[C:23]([C:25]([F:28])([F:27])[F:26])[CH:22]=[C:21]([C:29]4[CH:34]=[CH:33][C:32]([C:35]([F:38])([F:37])[F:36])=[CH:31][CH:30]=4)[N:20]=3)[CH:18]=2)=[N:11][C:10]=1[CH3:39])(=[O:8])=[O:7])(C)(C)C.C(O)(C(F)(F)F)=O>ClCCl>[CH3:39][C:10]1[N:11]=[C:12]([C:14]2[N:15]=[CH:16][N:17]([C:19]3[CH:24]=[C:23]([C:25]([F:28])([F:27])[F:26])[CH:22]=[C:21]([C:29]4[CH:30]=[CH:31][C:32]([C:35]([F:37])([F:36])[F:38])=[CH:33][CH:34]=4)[N:20]=3)[CH:18]=2)[S:13][C:9]=1[S:6]([NH2:5])(=[O:8])=[O:7]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 602094694-Methyl-2-{1-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-1H-imidazol-4-yl}-thiazole-5-sulfonic acid tert-butylamide

생성물 1

HCID 574690354-Methyl-2-{1-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-1H-imidazol-4-yl}-thiazole-5-sulfonic acid amide수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred and cooled suspension of 4-methyl-2-{1-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-1H-imidazol-4-yl}-thiazole-5-sulfonic acid tert-butylamide (example 292) (0.295 g, 0.50 mmol) in dichloromethane (3 mL) was added TFA (3 mL) and the reaction mixture was allowed to stir at room temperature for 16 h. The mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane were added. The mixture was stirred at room temperature for 1 h, the precipitate was collected by filtration, washed with water and heptane/diethyl ether and dried to yield the title compound as a white solid (0.264 g, 99%). MS (ISP) 534.2 [(M+H)+]; mp 187° C. (dec.).

후처리

  1. temperaturecooled
  2. stirringto stir at room temperature for 16 h
  3. customThe mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane
  4. additionwere added
  5. stirringThe mixture was stirred at room temperature for 1 h
  6. filtrationthe precipitate was collected by filtration
  7. washwashed with water and heptane/diethyl ether
  8. customdried

출처 및 근거

ORD 기록
ord-1ea2c26e43a84a9ea0626919c84600bc
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642264B2

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