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

HRID 454696
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인쇄 미리보기

반응식

HRID 454696 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매2회HCID 887Methanol용매
HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0347c22d1ea74f12bb0b0974687cf826
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08492582B2

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