Ethanol → (8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)-pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo-[1,5-a]pyridine mesylate

HRID 2369353노트

반응식

HRID 2369353 반응식
[S:1]([OH:5])(=[O:4])(=[O:3])[CH3:2].[CH3:6][O:7][C:8]1[N:13]=[C:12](/[CH:14]=[CH:15]/[C:16]2[N:34]=[C:19]3[C@H:20]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[C:30]([F:33])([F:32])[F:31])[CH2:21][CH2:22][CH2:23][N:18]3[N:17]=2)[CH:11]=[CH:10][C:9]=1[N:35]1[CH:39]=[C:38]([CH3:40])[N:37]=[CH:36]1.C(O)C>COC(C)(C)C>[S:1]([OH:5])(=[O:4])(=[O:3])[CH3:2].[CH3:6][O:7][C:8]1[N:13]=[C:12](/[CH:14]=[CH:15]/[C:16]2[N:34]=[C:19]3[C@H:20]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[C:30]([F:33])([F:32])[F:31])[CH2:21][CH2:22][CH2:23][N:18]3[N:17]=2)[CH:11]=[CH:10][C:9]=1[N:35]1[CH:39]=[C:38]([CH3:40])[N:37]=[CH:36]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 6395Methanesulfonic AcidHCID 46854987E-2212

생성물 1

HCID 46912967(8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)-pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo-[1,5-a]pyridine mesylate

시약·촉매·용매 1

HCID 15413tert-Butyl methyl ether용매

실험 절차

Mesylic acid (0.8 μL) was added to a mixed solution of (8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine (50 mg) in t-butyl methyl ether (0.8 mL)-ethanol (0.1 mL). The mixture was solidified as a result of stirring at room temperature for two hours. The solid was collected by filtration through a glass filter. The solid was washed with t-butyl methyl ether-ethanol (8:1) and then dried under reduced pressure at room temperature to obtain 51.9 mg of the title compound as pale yellow solid crystals.

후처리

  1. customa result
  2. filtrationThe solid was collected by filtration through a glass
  3. filtrationfilter
  4. washThe solid was washed with t-butyl methyl ether-ethanol (8:1)
  5. customdried under reduced pressure at room temperature

출처 및 근거

ORD 기록
ord-7593e2911b9f46e4b1b17c05086ea97c
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703954B2

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