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1-Naphthylamine → (3-Chloro-quinoxalin-2-yl)-naphthalen-1-yl-amine

HRID 44206
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HRID 44206 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.Cl[C:48]1[C:57]([Cl:58])=[N:56][C:55]2[C:50](=[CH:51][CH:52]=[CH:53][CH:54]=2)[N:49]=1.[C:59]1([NH2:69])[C:68]2[C:63](=[CH:64][CH:65]=[CH:66][CH:67]=2)[CH:62]=[CH:61][CH:60]=1.CC(C)([O-])C.[K+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:58][C:57]1[C:48]([NH:69][C:59]2[C:68]3[C:63](=[CH:64][CH:65]=[CH:66][CH:67]=3)[CH:62]=[CH:61][CH:60]=2)=[N:49][C:50]2[C:55]([N:56]=1)=[CH:54][CH:53]=[CH:52][CH:51]=2
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참가 물질

6

반응물 4

HCID 86401-NaphthylamineHCID 166592,3-DichloroquinoxalineHCID 634876Binap, (A+-)-HCID 23665647Potassium tert-butoxide

생성물 1

HCID 86656203(3-Chloro-quinoxalin-2-yl)-naphthalen-1-yl-amine수율 33%

시약·촉매·용매 1

HCID 167845
palladium(II) acetate
촉매

실험 절차

BINAP (93.3 mg, 0.15 mmol) and palladium acetate (22.6 mg, 0.1 mmol) were dissolved in dry xylenes (50 mL) and stirred for 10 min in an inert atmosphere of nitrogen. 2,3-Dichloroquinoxaline (1.99 g, 10 mmol), 1-naphthylamine (1.50 g, 10.5 mmol) and potassium tert-butoxide (1.34 g, 12 mmol) were the added to the reaction mixture which was heated for 22 h under reflux. After cooling to room-temperature, the reaction mixture was filtered and inorganic precipitate washed with dichloromethane (3×50 mL). Removal of the solvent in vacuo results in a residue which was purified using silica gel chromatography (hexanes/EtOAc 9:1). Compound 2c was isolated as yellow-orange crystals, mp=157-159° C. Yield 33%. TLC Rf=0.45 (hexanes/EtOAc 3:1). HPLC/MS: [M+H]+ m/z 306. 1H NMR (CDCl3, 600 MHz): δ 7.50 (td, J=7.2 Hz, 1.2 Hz, 1H), 7.56-7.63 (m, 4H), 7.74 (d, J=8.4 Hz, 1H), 7.78 (dd, J=8.4 Hz, 1.2 Hz, 1H), 7.89 (dd, J=8.4 Hz, 1.2 Hz, 1H), 7.90 (d, J=8.4 Hz, 1H), 7.99-8.04 (m, 2H), 8.54 (d, J=7.2 Hz, 1H). 13C NMR (CDCl3, 150 MHz): δ 118.62, 120.31, 125.01, 125.85, 126.10, 126.26, 126.45, 126.74, 126.79, 127.89, 129.01, 130.42, 133.25, 134.26, 137.25, 138.12, 140.59, 145.71. HRMS: Calcd. for C18H13ClN3 [M+H]+ m/z 306.0793, Observed 306.0786.

후처리

  1. additionadded to the reaction mixture which
  2. temperaturewas heated for 22 h
  3. temperatureunder reflux
  4. temperatureAfter cooling to room-temperature
  5. filtrationthe reaction mixture was filtered
  6. washinorganic precipitate washed with dichloromethane (3×50 mL)
  7. customRemoval of the solvent in vacuo
  8. customresults in a residue which
  9. customwas purified

출처 및 근거

ORD 기록
ord-a86ac29fa6964ebaa109712e06510298
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541415B2

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