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Benzene, 1-bromo-3-nitro- → HCID 67390544, 화합물

HRID 906214
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HRID 906214 반응식
C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.Br[C:48]1[CH:53]=[CH:52][CH:51]=[C:50]([N+:54]([O-:56])=[O:55])[CH:49]=1.Cl.Cl.[CH:59]([N:62]1[CH2:67][C@@H:66]2[CH2:68][C@H:63]1[CH2:64][NH:65]2)([CH3:61])[CH3:60].CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH:59]([N:62]1[CH2:67][C@@H:66]2[CH2:68][C@H:63]1[CH2:64][N:65]2[C:48]1[CH:53]=[CH:52][CH:51]=[C:50]([N+:54]([O-:56])=[O:55])[CH:49]=1)([CH3:61])[CH3:60]
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참가 물질

8

반응물 4

HCID 11457Benzene, 1-bromo-3-nitro-HCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 67389593(1S,4S)-2-(propan-2-yl)-2,5-diazabicyclo[2.2.1]heptane dihydrochloride

생성물 1

HCID 67390544HCID 67390544, 화합물수율 78.4%

시약·촉매·용매 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

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온도
40 °C

실험 절차

A solution of BINAP (0.47 g, 0.75 mmol) and tris(dibenzylideneacetone)dipalladium (0) (0.34 g, 0.37 mmol) in toluene (120 mL) was heated to 90° C. during 15 minutes under nitrogen. The reaction mixture was cooled to 40° C. before adding 1-bromo-3-nitrobenzene (1.89 g, 9.37 mmol), (1S,4S)-2-isopropyl-2,5-diazabicyclo[2.2.1]heptane dihydrochloride (2.0 g, 9.37 mmol) and sodium tert-butoxide (3.14 g, 32.74 mmol). The reaction was heated to 90° C. during 18 hours under nitrogen. After return to room temperature, the reaction was diluted with ethyl acetate and filtered through celite. The filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel eluting with a mixture of DCM/7N NH3 in methanol (96/4) to afford the title compound (1.92 g, 78%).

후처리

  1. temperatureThe reaction was heated to 90° C. during 18 hours under nitrogen
  2. filtrationfiltered through celite
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by flash chromatography on silica gel eluting with a mixture of DCM/7N NH3 in methanol (96/4)

출처 및 근거

ORD 기록
ord-5062982f87b649e18fdc2b7e7420f1f6
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08012983B2

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