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Hydrogen Bromide → (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 dihydrobromide

HRID 2369351
ノート
印刷プレビュー

反応式

HRID 2369351 の反応式
[BrH:1].[CH3:2][O:3][C:4]1[N:9]=[C:8](/[CH:10]=[CH:11]/[C:12]2[N:30]=[C:15]3[C@H:16]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]([F:29])([F:28])[F:27])[CH2:17][CH2:18][CH2:19][N:14]3[N:13]=2)[CH:7]=[CH:6][C:5]=1[N:31]1[CH:35]=[C:34]([CH3:36])[N:33]=[CH:32]1.CCCCCCC>C(O)C>[BrH:1].[BrH:1].[CH3:2][O:3][C:4]1[N:9]=[C:8](/[CH:10]=[CH:11]/[C:12]2[N:30]=[C:15]3[C@H:16]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]([F:29])([F:28])[F:27])[CH2:17][CH2:18][CH2:19][N:14]3[N:13]=2)[CH:7]=[CH:6][C:5]=1[N:31]1[CH:35]=[C:34]([CH3:36])[N:33]=[CH:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 260Hydrogen BromideHCID 8900Heptane2 回HCID 46854987E-2212

生成物 1

HCID 66991574(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 dihydrobromide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Concentrated hydrobromic acid (24.8 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 (51.42 mg) in ethanol (1 mL), and 1 mL of heptane was added with stirring at room temperature. After several minutes, 1 mL of heptane was further added to the solution and stirring was continued. The solution was stirred at room temperature for one hour and then further stirred at about 5° C. for 20 minutes. The precipitated solid was collected by filtration through a glass filter and dried under reduced pressure at room temperature to obtain 49.24 mg of the title compound as white solid crystals.

後処理

  1. additionwas added
  2. waitAfter several minutes
  3. stirringstirring
  4. stirringThe solution was stirred at room temperature for one hour
  5. stirringfurther stirred at about 5° C. for 20 minutes
  6. filtrationThe precipitated solid was collected by filtration through a glass
  7. filtrationfilter
  8. customdried under reduced pressure at room temperature

出典と根拠

ORDレコード
ord-4ff0de4d925a419daa5a0c4a91cb4f8b
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08703954B2

反応ノート

読み込み中…

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