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Potassium Phosphate, Tribasic → 2-(3-(quinolin-2-yl)phenoxy)-9H-carbazole

HRID 1509638
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HRID 1509638 반응식
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[CH:12]=[C:13]([OH:17])[CH:14]=[CH:15][CH:16]=1.I[C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[N+:31]([O-])=O)=[CH:21][CH:20]=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>[Cu]I.N1C=CC=CC=1C(O)=O>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[CH:12]=[C:13]([CH:14]=[CH:15][CH:16]=1)[O:17][C:19]1[CH:24]=[CH:23][C:22]2[C:25]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[NH:31][C:21]=2[CH:20]=1
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참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 6297494'-Iodo-2-nitrobiphenylHCID 14819923-(2-Quinolinyl)benzenol

생성물 1

HCID 1181142092-(3-(quinolin-2-yl)phenoxy)-9H-carbazole수율 101.1%

시약·촉매·용매 2

HCID 1018Picolinic acid촉매
HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매

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온도
85 °C

실험 절차

3-(quinolin-2-yl)phenol (3.68 g, 15.30 mmol, 1.0 eq), 4′-iodo-2-nitrobiphenyl (5.97 g, 18.36 mmol, 1.2 eq), CuI (0.15 g, 0.77 mmol, 0.05 eq), picolinic acid (0.19 g, 1.53 mmol, 0.1 eq) and K3PO4 (6.50 g, 30.60 mmol, 2.0 eq) were added to a dry pressure vessel equipped with a magnetic stir bar. The vessel was evacuated and back-filled with nitrogen. The evacuation and back-fill procedure was repeated twice. Then solvent DMSO (32 mL) was added under nitrogen. After bubbling with nitrogen for 20 minutes, the mixture was heated to 80-90° C. in an oil bath. The reaction was monitored by TLC and about 22 hours later the starting material 3-(quinolin-2-yl)phenol was consumed completely. Then the mixture was cooled to ambient temperature and diluted with water, extracted with ethyl acetate three times. The combined organic layer was washed with water three times and dried over sodium sulfate, and filtered and washed with ethyl acetate. The filtrate was concentrated and the residue was purified through column chromatography on silica gel using hexane and ethyl acetate (10:1-5:1-3:1) as an eluent to obtain the desired product as a sticky brown liquid (5.98 g), which was used directly for the next step. A solution of PPh3 (11.19 g, 42.6 mmol) and the sticky brown liquid (5.95 g) obtained in the last step in 1,2-dichlorobenzene (28.4 mL) was stirred at a temperature of 175-185° C. in oil bath and for 21 hours under nitrogen, cooled and the solvent was removed by distillation under high vacuum. The residue was purified through column chromatography on silica gel using hexane and ethyl acetate (10:1-5:1-3:1) as an eluent to obtain the desired product 2-(3-(quinolin-2-yl)phenoxy)-9H-carbazole, which was further purified through recrystallization in ethyl acetate and hexane to get pure product as a white solid (4.45 g) in 75% total yield for the four steps. 1H NMR (DMSO-d6, 400 MHz): δ 6.96 (dd, J=8.4, 2.4 Hz, 1H), 7.13 (d, J=2.4 Hz, 1H), 7.16 (d, J=7.6 Hz, 1H), 7.21 (dd, J=8.4, 2.4 Hz, 1H), 7.35 (d, J=8.0 Hz, 1H), 7.46 (d, J=8.0 Hz, 1H), 7.57-7.61 (m, 2H), 7.74-7.77 (m, 1H), 7.99-8.03 (m, 3H), 8.05-8.09 (m, 2H), 8.14 (d, J=5.6 Hz, 1H), 8.16 (d, J=5.2 Hz, 1H), 8.46 (d, J=9.2 Hz, 1H), 11.23 (s, 1H).

후처리

  1. customequipped with a magnetic stir bar
  2. customThe vessel was evacuated
  3. additionback-filled with nitrogen
  4. additionThen solvent DMSO (32 mL) was added under nitrogen
  5. customAfter bubbling with nitrogen for 20 minutes
  6. customwas monitored by TLC and about 22 hours
  7. customwas consumed completely
  8. temperatureThen the mixture was cooled to ambient temperature
  9. additiondiluted with water
  10. extractionextracted with ethyl acetate three times
  11. washThe combined organic layer was washed with water three times
  12. dry with materialdried over sodium sulfate
  13. filtrationfiltered
  14. washwashed with ethyl acetate
  15. concentrationThe filtrate was concentrated
  16. customthe residue was purified through column chromatography on silica gel

출처 및 근거

ORD 기록
ord-b800ddcac8654a2c9d58f361aa623655
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09224963B2

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