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Trimethylazanium;chloride → 1-(6-Chloro-3-hydroxypyridin-2-YL)ethan-1-one

HRID 2091260
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HRID 2091260 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[Cl-].C[NH+](C)C.C([O:17][C:18]1[C:19]([C:25](=[O:27])[CH3:26])=[N:20][C:21]([Cl:24])=[CH:22][CH:23]=1)C1C=CC=CC=1>C1(C)C=CC=CC=1>[Cl:24][C:21]1[N:20]=[C:19]([C:25](=[O:27])[CH3:26])[C:18]([OH:17])=[CH:23][CH:22]=1
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참가 물질

5

반응물 3

HCID 11649Trimethylazanium;chlorideHCID 6451240Aluminum(III) ChlorideHCID 866627441-[3-(Benzyloxy)-6-chloropyridin-2-yl]ethanone

생성물 1

HCID 722139671-(6-Chloro-3-hydroxypyridin-2-YL)ethan-1-one수율 86.1%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a suspension (80 mL) of aluminum chloride (14.3 g) in toluene was added trimethylammonium chloride (4.75 g), and the mixture was stirred under argon atmosphere at room temperature for 1 hr. To the mixture was added a solution (80 mL) of 1-[3-(benzyloxy)-6-chloropyridin-2-yl]ethanone (8.66 g) synthesized above in toluene, and the mixture was stirred at room temperature for 4 hr. The reaction mixture was concentrated under reduced pressure, saturated aqueous Rochelle salt solution was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane) to give the title object compound (4.89 g, 86%) as a pale-yellow solid.

후처리

  1. stirringthe mixture was stirred at room temperature for 4 hr
  2. concentrationThe reaction mixture was concentrated under reduced pressure, saturated aqueous Rochelle salt solution
  3. additionwas added to the residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-b51f280775f243eb8629cb46c0a7a802
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436043B2

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