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Sodium Carbonate → tert-Butyl 4-(2-nitrophenyl)-1,2,5,6-tetrahydropyridinecarboxylate

HRID 489643
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HRID 489643 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1B(O)O)([O-:3])=[O:2].[Li+].[Cl-].FC(F)(F)S(O[C:21]1[CH2:26][CH2:25][NH:24][CH:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH:22]=1)(=O)=O.C(OC(N1CCC(=O)CC1)=O)(C)(C)C.[Li+].CC([N-]C(C)C)C.C([O-])([O-])=O.[Na+].[Na+]>COCCOC.CCOC(C)=O>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:21]1[CH2:26][CH2:25][NH:24][CH:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH:22]=1)([O-:3])=[O:2]
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9

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HCID 10340Sodium CarbonateHCID 433294Lithium ChlorideHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 2724682Lithium diisopropylamideHCID 2773548(2-Nitrophenyl)boronic acidHCID 22266210Tert-butyl 4-[(trifluoromethyl)sulfonyloxy]-1,2,5,6-tetrahydropyridinecarboxylate

생성물 1

HCID 22266199tert-Butyl 4-(2-nitrophenyl)-1,2,5,6-tetrahydropyridinecarboxylate

시약·촉매·용매 2

HCID 80711,2-Dimethoxyethane용매HCID 8857Ethyl Acetate용매

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온도
90 °C

실험 절차

To a 100 mL round-bottomed flask equipped with stirring was added 2-nitrophenyl boronic acid (Combi-Blocks Chemical Company) (210 mg, 1.3 mmol), LiCl (Aldrich) (168 mg, 4 mmol), tetrakis(triphenyl-phosphine)palladium (O) (Strem Chemical Company) (69 mg, 0.06 mmol) and tert-butyl 4-[(trifluoromethyl)-sulfonyloxy]-1,2,5,6-tetrahydro-pyridinecarboxylate [prepared by the method of Wustrow, D. J. and Wise, L. D., Synthesis 1991, 993-995, from tert-butyl-4-oxopiperidine-1-carboxylate (Aldrich), LDA (Aldrich) and N-phenyltrifluoromethancsulfonimide (Aldrich)] (397 mg, 1.2 mmol) in DME (5 mL). The reaction mixture was purged with N2 and a 2 M soln of Na2CO3 (1.8 mL, 3.6 mmol) was introduced. After heating the mixture to 90° C. for 3 h, the reaction was cooled to 25° C. and diluted with EtOAc (15 mL). The organic layer was separated, washed with 10% Na2CO3, H2O and satd NaCl and dried over Na2SO4, filtered and concentrated in vacuo to afford a dark yellow oil. The crude material was purified by column chromatography (3:1 hexane:EtOAc) to give the title compound as a white solid (240 mg). MS (ESI, pos. ion) m/z: 305 (M+1). Calc'd for C16H20N2O4: 304.34.

후처리

  1. customTo a 100 mL round-bottomed flask equipped
  2. customprepared by the method of Wustrow, D
  3. custom, Synthesis 1991, 993-995
  4. customThe reaction mixture was purged with N2
  5. temperaturethe reaction was cooled to 25° C.
  6. customThe organic layer was separated
  7. washwashed with 10% Na2CO3, H2O
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customto afford a dark yellow oil
  12. customThe crude material was purified by column chromatography (3:1 hexane:EtOAc)

출처 및 근거

ORD 기록
ord-ca4b5f9ba6354ee08ad4f8a495404953
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06977264B2

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