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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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(6-Benzyloxy-pyridin-3-yloxy)-acetic acid ethyl ester → (6-Hydroxy-pyridin-3-yloxy)-acetic acid ethyl ester

HRID 417093
ノート
印刷プレビュー

反応式

HRID 417093 の反応式
[CH2:1]([O:3][C:4](=[O:21])[CH2:5][O:6][C:7]1[CH:8]=[N:9][C:10]([O:13]CC2C=CC=CC=2)=[CH:11][CH:12]=1)[CH3:2]>[Pd]>[CH2:1]([O:3][C:4](=[O:21])[CH2:5][O:6][C:7]1[CH:8]=[N:9][C:10]([OH:13])=[CH:11][CH:12]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 66619330(6-Benzyloxy-pyridin-3-yloxy)-acetic acid ethyl ester

生成物 1

HCID 178473014(6-Hydroxy-pyridin-3-yloxy)-acetic acid ethyl ester収率 91%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

The suspension of 0.64 g (2.23 mmol) (6-benzyloxy-pyridin-3-yloxy)-acetic acid ethyl ester and 0.064 g 10% palladium on charcoal was hydrogenated for 1 h at 1.7 bar. The reaction mixture was filtered over Dicalite Speed Plus, washed with ethanol and the filtrate was treated with silica gel and evaporated. The residue was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) with a gradient from heptane:ethyl acetate (100:0 to 0:100) followed by ethyl acetate:methanol (100:0 to 50:50) to give the product as a colorless solid (91%). MS (Turbo Spray): m/z=198.0 [M+H].

後処理

  1. filtrationThe reaction mixture was filtered over Dicalite Speed Plus
  2. washwashed with ethanol
  3. additionthe filtrate was treated with silica gel
  4. customevaporated
  5. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-5eee0917329147eb875c388903569cef
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088930B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート