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5-Acetyl-8-(benzyloxy)-1,2-dihydroquinolin-2-one → 8-Benzyloxy-5-(2-bromoacetyl)-2-hydroxyquinoline

HRID 332638
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HRID 332638 반응식
[C:1]([C:4]1[CH:13]=[CH:12][C:11]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:10]2[C:5]=1[CH:6]=[CH:7][C:8](=[O:22])[NH:9]2)(=[O:3])[CH3:2].[Br-:23].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1.CO>[CH2:15]([O:14][C:11]1[CH:12]=[CH:13][C:4]([C:1](=[O:3])[CH2:2][Br:23])=[C:5]2[C:10]=1[NH:9][C:8](=[O:22])[CH:7]=[CH:6]2)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
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참가 물질

5

반응물 2

HCID 133754445-Acetyl-8-(benzyloxy)-1,2-dihydroquinolin-2-oneHCID 23500184Tetra-n-butylammonium tribromide

생성물 1

HCID 116678678-Benzyloxy-5-(2-bromoacetyl)-2-hydroxyquinoline수율 73%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of 5-acetyl-8-(benzyloxy)quinolin-2(1H)-one (19.4 g, 66.4 mmol) in anhydrous THF (240 mL) and anhydrous methanol (165 mL) was added a solution of tetra-n-butylammonium tribromide (54.5 g, 113.0 mmol) in anhydrous THF (130 mL) dropwise over 1.5 hours. The resulting solution was stirred at RT overnight before concentrating under reduced pressure without heating. The residue was re-dissolved in methanol (200 mL). Saturated aqueous ammonium chloride solution (390 mL) was added with ice-cooling. The resulting suspension was filtered, and the solid washed with water and air-dried under vacuum. The solid was suspended in DCM and methanol (1:1 v/v, 100 mL) for 90 minutes. The solid was collected by filtration, washed with DCM and air-dried to afford the title compound (18.0 g, 73%).

후처리

  1. concentrationbefore concentrating under reduced pressure
  2. temperaturewithout heating
  3. dissolutionThe residue was re-dissolved in methanol (200 mL)
  4. additionSaturated aqueous ammonium chloride solution (390 mL) was added with ice-
  5. temperaturecooling
  6. filtrationThe resulting suspension was filtered
  7. washthe solid washed with water
  8. customair-dried under vacuum
  9. waitmethanol (1:1 v/v, 100 mL) for 90 minutes
  10. filtrationThe solid was collected by filtration
  11. washwashed with DCM
  12. customair-dried

출처 및 근거

ORD 기록
ord-7f5f73ac0f58484d8c90f3d9d86f6a45
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08877774B2

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