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1,4-Dioxane → Methyl 2-(5-(2-(azetidin-1-yl)ethoxy)-2-hydroxybenzamido)-4-phenylbenzoate

HRID 454696
ノート
印刷プレビュー

反応式

HRID 454696 の反応式
[N:1]1([CH2:5][CH2:6][O:7][C:8]2[CH:9]=[CH:10][C:11]([O:33]CC3C=CC=CC=3)=[C:12]([CH:32]=2)[C:13]([NH:15][C:16]2[CH:25]=[C:24]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH:23]=[CH:22][C:17]=2[C:18]([O:20][CH3:21])=[O:19])=[O:14])[CH2:4][CH2:3][CH2:2]1.O1CCOCC1>C(OCC)(=O)C.CO.[C].[Pd]>[N:1]1([CH2:5][CH2:6][O:7][C:8]2[CH:9]=[CH:10][C:11]([OH:33])=[C:12]([CH:32]=2)[C:13]([NH:15][C:16]2[CH:25]=[C:24]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH:23]=[CH:22][C:17]=2[C:18]([O:20][CH3:21])=[O:19])=[O:14])[CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 312751,4-DioxaneHCID 66990372Methyl 2-(5-(2-(azetidin-1-yl)ethoxy)-2-(benzyloxy)benzamido)-4-phenylbenzoate

生成物 1

HCID 58508869Methyl 2-(5-(2-(azetidin-1-yl)ethoxy)-2-hydroxybenzamido)-4-phenylbenzoate収率 45.1%

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒2 回HCID 887Methanol溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

To a solution mixture of the obtained methyl 2-(5-(2-(azetidin-1-yl)ethoxy)-2-(benzyloxy)benzamido)-4-phenylbenzoate (0.088 g) in ethyl acetate (1.5 mL), methanol (1.5 mL), and dioxane (1.5 mL), 10% palladium-carbon (0.088 g) was added, followed by stirring under a hydrogen atmosphere at room temperature for 2 hours. To the reaction mixture, 10% palladium-carbon (0.088 g) was added, followed by stirring under a hydrogen atmosphere at room temperature for 3 hours. The insoluble substance was removed by filtration, and then the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.033 g of methyl 2-(5-(2-(azetidin-1-yl)ethoxy)-2-hydroxybenzamido)-4-phenylbenzoate as a light yellow solid.

後処理

  1. additionwas added
  2. stirringby stirring under a hydrogen atmosphere at room temperature for 3 hours
  3. customThe insoluble substance was removed by filtration
  4. customthe solvent was evaporated under reduced pressure
  5. additionDiisopropyl ether was added to the obtained residue
  6. filtrationthe solid substance was collected by filtration

出典と根拠

ORDレコード
ord-0347c22d1ea74f12bb0b0974687cf826
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492582B2

反応ノート

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