Sulfuric Acid → (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 disulfate

HRID 2369350ノート

反応式

HRID 2369350 の反応式
[S:1](=[O:5])(=[O:4])([OH:3])[OH: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(OCC)(=O)C>C(O)C>[S:1]([O:3][S:1]([OH:4])(=[O:3])=[O:2])([OH:2])(=[O:5])=[O:4].[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 1118Sulfuric AcidHCID 8857Ethyl AcetateHCID 46854987E-2212

生成物 1

HCID 66990750(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 disulfate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Concentrated sulfuric acid (11.5 μL) was added to a 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 (98.09 mg) in ethanol (1 mL), and 1 mL of ethyl acetate was added with stirring at room temperature. Since the oily portion was confirmed on the bottom of the recovery flask, the oily substance was dissolved by ultrasonic treatment. Stirring at room temperature under shading for about 30 minutes resulted in precipitation of a solid. The solid was collected by filtration through a glass filter and dried under reduced pressure at room temperature to obtain 127.94 mg of the title compound as white solid crystals.

後処理

  1. additionwas added
  2. dissolutionthe oily substance was dissolved by ultrasonic treatment
  3. stirringStirring at room temperature under shading for about 30 minutes
  4. customresulted in precipitation of a solid
  5. filtrationThe solid was collected by filtration through a glass
  6. filtrationfilter
  7. customdried under reduced pressure at room temperature

出典と根拠

ORDレコード
ord-568566e960fb46ab99581cd931321093
出典データセット
uspto-grants-2014_04
特許番号
US08703954B2

反応ノート

読み込み中…