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 2369353ノート

反応式

HRID 2369353 の反応式
[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

参加物

5

反応物 3

HCID 702EthanolHCID 6395Methanesulfonic AcidHCID 46854987E-2212

生成物 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

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7593e2911b9f46e4b1b17c05086ea97c
出典データセット
uspto-grants-2014_04
特許番号
US08703954B2

反応ノート

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