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Acetic Acid → 5-Amino-6-((S)-2-imidazol-1-yl-1-pyridin-3-yl-ethoxy)-3,4-dihydro-2H-naphthalen-1-one

HRID 496429
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HRID 496429 반응식
[N:1]1([CH2:6][C@H:7]([C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[O:8][C:9]2[C:10]([N+:20]([O-])=O)=[C:11]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[CH2:14][CH2:13][CH2:12]3)[CH:5]=[CH:4][N:3]=[CH:2]1.CO.C(O)(=O)C.C([O-])(O)=O.[Na+]>[Fe].CCOC(C)=O.O>[NH2:20][C:10]1[C:9]([O:8][C@@H:7]([C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[CH2:6][N:1]2[CH:5]=[CH:4][N:3]=[CH:2]2)=[CH:18][CH:17]=[C:16]2[C:11]=1[CH2:12][CH2:13][CH2:14][C:15]2=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 516892Sodium BicarbonateHCID 697370746-((S)-2-Imidazol-1-yl-1-pyridin-3-yl-ethoxy)-5-nitro-3,4-dihydro-2H-naphthalen-1-one

생성물 1

HCID 697352345-Amino-6-((S)-2-imidazol-1-yl-1-pyridin-3-yl-ethoxy)-3,4-dihydro-2H-naphthalen-1-one수율 46.6%

시약·촉매·용매 3

HCID 23925
Iron
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 6-((S)-2-Imidazol-1-yl-1-pyridin-3-yl-ethoxy)-5-nitro-3,4-dihydro-2H-naphthalen-1-one (1.60 g, 4.23 mmol), MeOH (85 mL), H2O (19 mL) and glacial acetic acid (2.4 mL, 42 mmol) was treated at reflux with iron powder (2.34 g, 42 mmol). The reaction was monitored by mass spectrometry and was complete in 4 h. The volume of solvent was reduced under reduced pressure. EtOAc and dilute aqueous NaHCO3 were added. A brownish-green emulsion formed which was filtered through Celite. The mixture was extracted with EtOAc. The combined organic layer was washed with dilute aqueous NaHCO3 and brine, dried over Na2SO4, and concentrated under reduced pressure to give an off-white foam (0.685 g, 1.97 mmol, 46%). The structure was confirmed by NMR and mass spectrometry. MS m/z 349 (M++H).

후처리

  1. additionwas treated
  2. customA brownish-green emulsion formed which
  3. filtrationwas filtered through Celite
  4. extractionThe mixture was extracted with EtOAc
  5. washThe combined organic layer was washed with dilute aqueous NaHCO3 and brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6e1990f2a90e4710b89d79cebe27b6ce
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06943183B2

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