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Phosphorus tribromide → 1-[2-(4-Bromomethyl-phenyl)-ethyl]-4-phenethyl-1H-pyridin-2-one

HRID 564159
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반응식

HRID 564159 반응식
O[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:13][C:12]2=[O:25])=[CH:5][CH:4]=1.P(Br)(Br)[Br:27].C([O-])(O)=O.[Na+]>C(Cl)Cl>[Br:27][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:13][C:12]2=[O:25])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24614Phosphorus tribromideHCID 516892Sodium BicarbonateHCID 670073171-[2-(4-Hydroxymethyl-phenyl)-ethyl]-4-phenethyl-1H-pyridin-2-one

생성물 1

HCID 670066581-[2-(4-Bromomethyl-phenyl)-ethyl]-4-phenethyl-1H-pyridin-2-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 150 mg (0.45 mmol) 1-[2-(4-hydroxymethyl-phenyl)-ethyl]-4-phenethyl-1H-pyridin-2-one (example 18.1a) in 2.0 mL of DCM is added at 0° C. 21 μL (0.23 mmol) phosphorus tribromide. The mixture is stirred 2 h at RT and is then added to aqueous 5% NaHCO3-solution. The layers are separated, the aqueous phase is extracted with DCM. The combined organic phase is washed with water, dried over MgSO4, filtered and the solvent is evaporated to afford the product.

후처리

  1. customThe layers are separated
  2. extractionthe aqueous phase is extracted with DCM
  3. washThe combined organic phase is washed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent is evaporated
  7. customto afford the product

출처 및 근거

ORD 기록
ord-5173d15553f64107be5b637eaea21d87
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08067590B2

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