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Trifluoroacetic acid → (5-fluoro-2-methoxy-pyridin-3-ylmethyl)-[3-methoxy-5-(5-methyl-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-yl]-amine

HRID 509977
ノート
印刷プレビュー

反応式

HRID 509977 の反応式
[CH3:1][O:2][C:3]1[C:4]([NH2:20])=[N:5][CH:6]=[C:7]([CH2:9][C:10]2[C:18]3[C:13](=[N:14][CH:15]=[C:16]([CH3:19])[CH:17]=3)[NH:12][CH:11]=2)[CH:8]=1.[F:21][C:22]1[CH:23]=[C:24]([CH:30]=O)[C:25]([O:28][CH3:29])=[N:26][CH:27]=1.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>C(#N)C>[F:21][C:22]1[CH:23]=[C:24]([CH2:30][NH:20][C:4]2[C:3]([O:2][CH3:1])=[CH:8][C:7]([CH2:9][C:10]3[C:18]4[C:13](=[N:14][CH:15]=[C:16]([CH3:19])[CH:17]=4)[NH:12][CH:11]=3)=[CH:6][N:5]=2)[C:25]([O:28][CH3:29])=[N:26][CH:27]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 226783235-Fluoro-2-methoxynicotinaldehydeHCID 582593253-methoxy-5-(5-methyl-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-ylamine

生成物 1

HCID 67200110(5-fluoro-2-methoxy-pyridin-3-ylmethyl)-[3-methoxy-5-(5-methyl-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-yl]-amine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

To 3-methoxy-5-(5-methyl-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-ylamine (128, 1 equivalent) in 2 mL of acetonitrile, 5-fluoro-2-methoxy-pyridine-3-carbaldehyde (37, 1 equivalent), triethylsilane (5 equivalents) and trifluoroacetic acid (6.9 equivalents) are added. The reaction is heated at 80° C. for 18 hours, then concentrated under vacuum and mixed with aqueous potassium carbonate and extracted with ethyl acetate. The organic layer is washed with water, brine, then dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography eluting with ethyl acetate and hexane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound.

後処理

  1. concentrationconcentrated under vacuum
  2. additionmixed with aqueous potassium carbonate
  3. extractionextracted with ethyl acetate
  4. washThe organic layer is washed with water, brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated under vacuum
  8. customThe resulting material is purified by silica gel column chromatography
  9. washeluting with ethyl acetate and hexane
  10. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-2060f99c2fbc4491ac5e8919d476ca23
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096593B2

反応ノート

読み込み中…

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